Chinese Journal of Chromatography ›› 2022, Vol. 40 ›› Issue (5): 409-422.DOI: 10.3724/SP.J.1123.2021.12005
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FENG Yuechao, WANG Jianfeng, HOU Fan, DING Qi, CHU Hongyu, LIU Yan()
Received:
2021-12-27
Online:
2022-05-08
Published:
2022-04-28
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LIU Yan
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FENG Yuechao, WANG Jianfeng, HOU Fan, DING Qi, CHU Hongyu, LIU Yan. Determination of 44 foodborne stimulants and 6 progestogens in meat by QuEChERS and ultra-performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2022, 40(5): 409-422.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2021.12005
No. | Compound | Retention time/min | Parent ion (m/z) | Quantitative/ qualitative ions (m/z) | Collision voltages/V | Cone voltage/V |
---|---|---|---|---|---|---|
1 | tulobuterol (妥布特罗) | 4.97 | 228.4 | 172.2/154.1 | 10/16 | 18 |
2 | clenbuterol (克伦特罗) | 4.56 | 277.4 | 132.1/203.1 | 26/14 | 34 |
3 | bambuterol (班布特罗) | 5.12 | 368.7 | 72.2/294.4 | 34/20 | 18 |
4 | salmeterol (沙美特罗) | 7.31 | 416.7 | 91.2/380.6 | 38/18 | 25 |
5 | clenproperol (克伦丙罗) | 2.83 | 263.3 | 203.1/168.1 | 16/26 | 26 |
6 | zilpaterol (齐帕特罗) | 2.82 | 262.4 | 185.2/202.2 | 24/18 | 18 |
7 | fenoterol (菲诺特罗) | 3.37 | 304.5 | 107.2/135.2 | 30/16 | 4 |
8 | penbuterol (喷布特罗) | 7.31 | 292.5 | 236.3/74.2 | 14/20 | 72 |
9 | clencyclohexerol (克伦塞罗) | 3.81 | 319.4 | 203.1/81.1 | 20/26 | 36 |
10 | mabuterol (马布特罗) | 5.02 | 311.4 | 217.2/237.2 | 24/14 | 20 |
11 | brombuterol (溴布特罗) | 4.96 | 367.4 | 132.3/293.1 | 46/18 | 26 |
12 | cimaterol (西马特罗) | 2.64 | 220.4 | 160.2/143.2 | 14/24 | 18 |
13 | salbutamol (沙丁胺醇) | 2.86 | 240.4 | 148.2/166.2 | 16/12 | 16 |
14 | metaproterenol (奥西那林) | 2.20 | 212.3 | 152.1/125.2 | 16/20 | 22 |
15 | terbutaline (特布他林) | 2.80 | 226.4 | 152.2/125.1 | 14/22 | 30 |
16 | clorprenaline (氯丙那林) | 4.51 | 214.3 | 154.2/118.9 | 16/26 | 18 |
17 | ractopamine (莱克多巴胺) | 4.21 | 302.5 | 107.2/164.2 | 26/14 | 26 |
18 | demethyl coclaurine (去甲乌药碱) | 3.32 | 272.4 | 107.2/161.2 | 20/18 | 40 |
19 | tretoquinol (曲托喹酚) | 4.22 | 346.5 | 149.1/164.2 | 50/14 | 6 |
20 | atenolol (阿替洛尔) | 2.87 | 267.4 | 145.2/74.2 | 26/22 | 20 |
21 | propranolol (普萘洛尔) | 5.94 | 260.4 | 183.2/116.2 | 18/16 | 18 |
22 | metoprolol (美托洛尔) | 4.75 | 268.5 | 72.1/116.2 | 18/18 | 18 |
23 | trenbolone (群勃龙) | 6.98 | 271.4 | 199.2/165.3 | 22/44 | 62 |
24 | methyltestosterone (甲基睾酮) | 7.75 | 303.6 | 97.1/109.2 | 26/24 | 32 |
25 | boldenone (勃地酮) | 7.06 | 287.5 | 121.1/135.2 | 26/14 | 30 |
26 | nortestosterone (诺龙) | 7.20 | 275.1 | 109.0/257.2 | 28/16 | 2 |
27 | stanozolol (司坦唑醇) | 8.33 | 329.6 | 81.1/95.1 | 38/38 | 16 |
28 | methandienone (去氢甲睾酮) | 7.31 | 301.5 | 121.1/149.2 | 26/14 | 26 |
29 | mesterolone (美睾酮) | 8.33 | 305.5 | 269.4/95.6 | 16/32 | 15 |
30 | mestanolone (美雄诺龙) | 8.45 | 305.6 | 269.4/105.2 | 14/20 | 10 |
31 | testosterone (睾酮) | 7.49 | 289.5 | 97.1/109.2 | 20/22 | 48 |
32 | 4-androstene-3 (雄烯二酮) | 7.19 | 287.5 | 97.2/109.2 | 20/24 | 34 |
33 | prasterone (脱氢表雄酮) | 7.49 | 289.5 | 253.3/213.3 | 10/18 | 6 |
34 | progesterone (孕酮) | 8.40 | 315.5 | 97.1/109.2 | 20/22 | 12 |
35 | chlormadinone acetate (醋酸氯地孕酮) | 8.20 | 405.1 | 309.1/345.1 | 16/14 | 4 |
36 | melengestrol acetate (醋酸美伦孕酮) | 8.30 | 397.2 | 279.2/337.1 | 22/14 | 2 |
37 | medroxyprogesterone acetate (醋酸甲羟孕酮) | 8.25 | 387.2 | 123.0/327.2 | 32/14 | 2 |
38 | 17-α-hydroxyprogesterone (17-α-羟孕酮) | 7.58 | 331.2 | 97.0/109.2 | 26/30 | 4 |
39 | megestrol (甲地孕酮) | 7.87 | 343.1 | 187.1/325.1 | 26/18 | 2 |
No. | Compound | Retention time/min | Parent ion (m/z) | Quantitative/ qualitative ions (m/z) | Collision voltages/V | Cone voltage/V |
40 | triamterene (氨苯喋啶) | 4.43 | 254.4 | 141.1/104.2 | 44/38 | 16 |
41 | spironolactone (螺内酯) | 7.10 | 341.5 | 107.2/91.1 | 26/48 | 48 |
42 | canrenone (坎利酮) | 7.11 | 341.5 | 107.2/91.1 | 28/52 | 58 |
43 | dexamethasone (地塞米松) | 6.78 | 393.5 | 373.4/355.3 | 8/10 | 12 |
44 | hydrocortisone (氢化可的松) | 6.42 | 363.5 | 121.1/105.1 | 22/44 | 44 |
45 | prednisolone (波尼松龙) | 6.42 | 361.5 | 325.4/307.4 | 8/10 | 24 |
46 | cortisone (可的松) | 6.19 | 361.6 | 163.2/121.2 | 24/36 | 18 |
47 | prednisone (泼尼松) | 6.11 | 359.5 | 147.1/313.4 | 26/12 | 28 |
48 | fluocinolone acetonide (醋酸氟轻松) | 6.82 | 453.5 | 121.2/433.4 | 28/8 | 16 |
49 | fludrocortisone (氟氢可的松) | 6.34 | 381.5 | 239.3/91.2 | 24/58 | 38 |
50 | beclomethasone (倍氯米松) | 6.81 | 409.5 | 373.4/121.2 | 8/42 | 6 |
I-1 | methyltestosterone-D3 (甲基睾酮-D3) | 7.90 | 306.6 | 97.2/109.2 | 24/28 | 10 |
I-2 | testosterone-D3 (睾酮-D3) | 7.49 | 292.5 | 97.2/109.1 | 24/20 | 90 |
I-3 | hydrocortisone-D3 (氢化可的松-D3) | 6.42 | 366.6 | 121.2/330.4 | 22/14 | 16 |
I-4 | salbutamol-D3 (沙丁胺醇-D3) | 2.85 | 243.5 | 151.2/169.2 | 16/12 | 32 |
I-5 | boldenone--D3 (勃地酮-D3) | 7.05 | 290.6 | 121.2/138.1 | 22/12 | 12 |
I-6 | clenbuterol-D9 (克伦特罗-D9) | 4.54 | 286.4 | 204.1/133.0 | 16/28 | 6 |
I-7 | dexamethasone-D5 (地塞米松-D5) | 6.78 | 398.6 | 378.5/360.4 | 8/10 | 12 |
I-8 | ractopamine-D5 (莱克多巴胺-D5) | 4.19 | 307.5 | 165.2/111.1 | 14/32 | 14 |
I-9 | progesterone-D9 (孕酮-D9) | 8.35 | 324.6 | 100.1/113.2 | 20/24 | 26 |
I-10 | demethyl coclaurine-D4 (去甲乌药碱-D4) | 3.28 | 276.5 | 108.3/164.3 | 20/18 | 18 |
I-11 | tretoquinol-D9 (曲托喹酚-D9) | 4.18 | 355.6 | 164.1/137.1 | 16/46 | 12 |
Table 1 Retention times and MS parameters for 50 target analytes and 11 isotope internal standard compounds
No. | Compound | Retention time/min | Parent ion (m/z) | Quantitative/ qualitative ions (m/z) | Collision voltages/V | Cone voltage/V |
---|---|---|---|---|---|---|
1 | tulobuterol (妥布特罗) | 4.97 | 228.4 | 172.2/154.1 | 10/16 | 18 |
2 | clenbuterol (克伦特罗) | 4.56 | 277.4 | 132.1/203.1 | 26/14 | 34 |
3 | bambuterol (班布特罗) | 5.12 | 368.7 | 72.2/294.4 | 34/20 | 18 |
4 | salmeterol (沙美特罗) | 7.31 | 416.7 | 91.2/380.6 | 38/18 | 25 |
5 | clenproperol (克伦丙罗) | 2.83 | 263.3 | 203.1/168.1 | 16/26 | 26 |
6 | zilpaterol (齐帕特罗) | 2.82 | 262.4 | 185.2/202.2 | 24/18 | 18 |
7 | fenoterol (菲诺特罗) | 3.37 | 304.5 | 107.2/135.2 | 30/16 | 4 |
8 | penbuterol (喷布特罗) | 7.31 | 292.5 | 236.3/74.2 | 14/20 | 72 |
9 | clencyclohexerol (克伦塞罗) | 3.81 | 319.4 | 203.1/81.1 | 20/26 | 36 |
10 | mabuterol (马布特罗) | 5.02 | 311.4 | 217.2/237.2 | 24/14 | 20 |
11 | brombuterol (溴布特罗) | 4.96 | 367.4 | 132.3/293.1 | 46/18 | 26 |
12 | cimaterol (西马特罗) | 2.64 | 220.4 | 160.2/143.2 | 14/24 | 18 |
13 | salbutamol (沙丁胺醇) | 2.86 | 240.4 | 148.2/166.2 | 16/12 | 16 |
14 | metaproterenol (奥西那林) | 2.20 | 212.3 | 152.1/125.2 | 16/20 | 22 |
15 | terbutaline (特布他林) | 2.80 | 226.4 | 152.2/125.1 | 14/22 | 30 |
16 | clorprenaline (氯丙那林) | 4.51 | 214.3 | 154.2/118.9 | 16/26 | 18 |
17 | ractopamine (莱克多巴胺) | 4.21 | 302.5 | 107.2/164.2 | 26/14 | 26 |
18 | demethyl coclaurine (去甲乌药碱) | 3.32 | 272.4 | 107.2/161.2 | 20/18 | 40 |
19 | tretoquinol (曲托喹酚) | 4.22 | 346.5 | 149.1/164.2 | 50/14 | 6 |
20 | atenolol (阿替洛尔) | 2.87 | 267.4 | 145.2/74.2 | 26/22 | 20 |
21 | propranolol (普萘洛尔) | 5.94 | 260.4 | 183.2/116.2 | 18/16 | 18 |
22 | metoprolol (美托洛尔) | 4.75 | 268.5 | 72.1/116.2 | 18/18 | 18 |
23 | trenbolone (群勃龙) | 6.98 | 271.4 | 199.2/165.3 | 22/44 | 62 |
24 | methyltestosterone (甲基睾酮) | 7.75 | 303.6 | 97.1/109.2 | 26/24 | 32 |
25 | boldenone (勃地酮) | 7.06 | 287.5 | 121.1/135.2 | 26/14 | 30 |
26 | nortestosterone (诺龙) | 7.20 | 275.1 | 109.0/257.2 | 28/16 | 2 |
27 | stanozolol (司坦唑醇) | 8.33 | 329.6 | 81.1/95.1 | 38/38 | 16 |
28 | methandienone (去氢甲睾酮) | 7.31 | 301.5 | 121.1/149.2 | 26/14 | 26 |
29 | mesterolone (美睾酮) | 8.33 | 305.5 | 269.4/95.6 | 16/32 | 15 |
30 | mestanolone (美雄诺龙) | 8.45 | 305.6 | 269.4/105.2 | 14/20 | 10 |
31 | testosterone (睾酮) | 7.49 | 289.5 | 97.1/109.2 | 20/22 | 48 |
32 | 4-androstene-3 (雄烯二酮) | 7.19 | 287.5 | 97.2/109.2 | 20/24 | 34 |
33 | prasterone (脱氢表雄酮) | 7.49 | 289.5 | 253.3/213.3 | 10/18 | 6 |
34 | progesterone (孕酮) | 8.40 | 315.5 | 97.1/109.2 | 20/22 | 12 |
35 | chlormadinone acetate (醋酸氯地孕酮) | 8.20 | 405.1 | 309.1/345.1 | 16/14 | 4 |
36 | melengestrol acetate (醋酸美伦孕酮) | 8.30 | 397.2 | 279.2/337.1 | 22/14 | 2 |
37 | medroxyprogesterone acetate (醋酸甲羟孕酮) | 8.25 | 387.2 | 123.0/327.2 | 32/14 | 2 |
38 | 17-α-hydroxyprogesterone (17-α-羟孕酮) | 7.58 | 331.2 | 97.0/109.2 | 26/30 | 4 |
39 | megestrol (甲地孕酮) | 7.87 | 343.1 | 187.1/325.1 | 26/18 | 2 |
No. | Compound | Retention time/min | Parent ion (m/z) | Quantitative/ qualitative ions (m/z) | Collision voltages/V | Cone voltage/V |
40 | triamterene (氨苯喋啶) | 4.43 | 254.4 | 141.1/104.2 | 44/38 | 16 |
41 | spironolactone (螺内酯) | 7.10 | 341.5 | 107.2/91.1 | 26/48 | 48 |
42 | canrenone (坎利酮) | 7.11 | 341.5 | 107.2/91.1 | 28/52 | 58 |
43 | dexamethasone (地塞米松) | 6.78 | 393.5 | 373.4/355.3 | 8/10 | 12 |
44 | hydrocortisone (氢化可的松) | 6.42 | 363.5 | 121.1/105.1 | 22/44 | 44 |
45 | prednisolone (波尼松龙) | 6.42 | 361.5 | 325.4/307.4 | 8/10 | 24 |
46 | cortisone (可的松) | 6.19 | 361.6 | 163.2/121.2 | 24/36 | 18 |
47 | prednisone (泼尼松) | 6.11 | 359.5 | 147.1/313.4 | 26/12 | 28 |
48 | fluocinolone acetonide (醋酸氟轻松) | 6.82 | 453.5 | 121.2/433.4 | 28/8 | 16 |
49 | fludrocortisone (氟氢可的松) | 6.34 | 381.5 | 239.3/91.2 | 24/58 | 38 |
50 | beclomethasone (倍氯米松) | 6.81 | 409.5 | 373.4/121.2 | 8/42 | 6 |
I-1 | methyltestosterone-D3 (甲基睾酮-D3) | 7.90 | 306.6 | 97.2/109.2 | 24/28 | 10 |
I-2 | testosterone-D3 (睾酮-D3) | 7.49 | 292.5 | 97.2/109.1 | 24/20 | 90 |
I-3 | hydrocortisone-D3 (氢化可的松-D3) | 6.42 | 366.6 | 121.2/330.4 | 22/14 | 16 |
I-4 | salbutamol-D3 (沙丁胺醇-D3) | 2.85 | 243.5 | 151.2/169.2 | 16/12 | 32 |
I-5 | boldenone--D3 (勃地酮-D3) | 7.05 | 290.6 | 121.2/138.1 | 22/12 | 12 |
I-6 | clenbuterol-D9 (克伦特罗-D9) | 4.54 | 286.4 | 204.1/133.0 | 16/28 | 6 |
I-7 | dexamethasone-D5 (地塞米松-D5) | 6.78 | 398.6 | 378.5/360.4 | 8/10 | 12 |
I-8 | ractopamine-D5 (莱克多巴胺-D5) | 4.19 | 307.5 | 165.2/111.1 | 14/32 | 14 |
I-9 | progesterone-D9 (孕酮-D9) | 8.35 | 324.6 | 100.1/113.2 | 20/24 | 26 |
I-10 | demethyl coclaurine-D4 (去甲乌药碱-D4) | 3.28 | 276.5 | 108.3/164.3 | 20/18 | 18 |
I-11 | tretoquinol-D9 (曲托喹酚-D9) | 4.18 | 355.6 | 164.1/137.1 | 16/46 | 12 |
Fig. 2 Percentages of compounds with recoveries greater than 50%, using an extraction solution of acetonitrile containing different proportions of acetic acid in the chicken matrix
Fig. 3 Percentages of target compounds in total analytes within different ranges of recoveries using different purifying agents in the chicken matrix ① PSA 250 mg+C18 250 mg; ② PSA 250 mg+neutral alumina 250 mg; ③ C18 250 mg+neutral alumina 250 mg; ④ PSA 165 mg+C18 165 mg+neutral alumina 165 mg.
No. | Compound | Internal standard* | Linear range/ (μg/L) | Linear equation | R2 | LOD/ (μg/kg) | LOQ/ (μg/kg) | SSE/ % |
---|---|---|---|---|---|---|---|---|
1 | tulobuterol | clenbuterol-D9 | 0.1-20 | y=1.008x+0.0127 | 0.9992 | 0.03 | 0.1 | 109 |
2 | clenbuterol | clenbuterol-D9 | 0.1-20 | y=1.259x+0.0982 | 0.9994 | 0.03 | 0.1 | 97 |
3 | bambuterol | clenbuterol-D9 | 0.1-20 | y=0.415x-0.0548 | 0.9995 | 0.03 | 0.1 | 148 |
4 | salmeterol | ractopamine-D5 | 0.1-20 | y=0.339x-0.0420 | 0.9980 | 0.03 | 0.1 | 133 |
5 | clenproperol | clenbuterol-D9 | 0.2-20 | y=0.725x+0.0577 | 0.9992 | 0.07 | 0.2 | 108 |
6 | zilpaterol | salbutamol-D3 | 0.1-20 | y=0.921x+0.163 | 0.9975 | 0.03 | 0.1 | 85 |
7 | fenoterol | salbutamol-D3 | 0.1-20 | y=1.119x-0.0307 | 0.9992 | 0.03 | 0.1 | 104 |
8 | penbuterol | clenbuterol-D9 | 0.1-10 | y=4.360x+0.259 | 0.9961 | 0.03 | 0.1 | 129 |
9 | clencyclohexerol | clenbuterol-D9 | 0.1-20 | y=1.324x+0.132 | 0.9985 | 0.03 | 0.1 | 80 |
10 | mabuterol | clenbuterol-D9 | 0.2-20 | y=0.116x+0.00952 | 0.9991 | 0.07 | 0.2 | 108 |
11 | brombuterol | clenbuterol-D9 | 0.1-20 | y=0.137x-0.00338 | 0.9993 | 0.03 | 0.1 | 124 |
12 | cimaterol | clenbuterol-D9 | 0.2-20 | y=1.042x+0.0599 | 0.9996 | 0.07 | 0.2 | 117 |
13 | salbutamol | salbutamol-D3 | 0.1-10 | y=0.432x+0.0494 | 0.9971 | 0.03 | 0.1 | 105 |
14 | metaproterenol | clenbuterol-D9 | 0.1-20 | y=2.046x-0.0725 | 0.9993 | 0.03 | 0.1 | 103 |
15 | terbutaline | clenbuterol-D9 | 0.1-10 | y=3.548x+0.159 | 0.9987 | 0.03 | 0.1 | 138 |
16 | clorprenaline | clenbuterol-D9 | 0.1-20 | y=0.752x+0.0253 | 0.9997 | 0.03 | 0.1 | 177 |
17 | ractopamine | ractopamine-D5 | 0.1-20 | y=1.121x+0.390 | 0.9989 | 0.03 | 0.1 | 92 |
18 | demethyl coclaurine | demethyl coclaurine-D4 | 0.1-10 | y=3.200x+0.0441 | 0.9999 | 0.03 | 0.1 | 92 |
19 | tretoquinol | tretoquinol-D9 | 0.1-20 | y=0.146x-0.00404 | 0.9994 | 0.03 | 0.1 | 115 |
20 | atenolol | clenbuterol-D9 | 0.1-20 | y=1.789x+0.333 | 0.9959 | 0.03 | 0.1 | 127 |
21 | propranolol | clenbuterol-D9 | 0.1-20 | y=1.761x+0.0714 | 0.9996 | 0.03 | 0.1 | 87 |
22 | metoprolol | clenbuterol-D9 | 0.1-20 | y=1.137x+0.0171 | 0.9999 | 0.03 | 0.1 | 75 |
23 | trenbolone | boldenone-D3 | 0.2-50 | y=2.423x+1.230 | 0.9951 | 0.07 | 0.2 | 112 |
24 | methyltestosterone | methyltestosterone-D3 | 0.2-50 | y=0.737x+0.175 | 0.9957 | 0.07 | 0.2 | 90 |
25 | boldenone | boldenone-D3 | 0.2-50 | y=3.571x+0.923 | 0.9971 | 0.07 | 0.2 | 85 |
26 | nortestosterone | testosterone-D3 | 0.2-50 | y=0.0158x+0.0105 | 0.9963 | 0.07 | 0.2 | 106 |
27 | stanozolol | progesterone-D9 | 0.2-50 | y=1.858x-0.138 | 0.9987 | 0.07 | 0.2 | 103 |
28 | methandienone | testosterone-D3 | 0.2-50 | y=0.022x+0.0111 | 0.9951 | 0.07 | 0.2 | 95 |
29 | mesterolone | methyltestosterone-D3 | 0.2-50 | y=0.0284x+0.0152 | 0.9966 | 0.07 | 0.2 | 173 |
30 | mestanolone | methyltestosterone-D3 | 0.2-50 | y=0.0274x-0.0303 | 0.9957 | 0.07 | 0.2 | 95 |
31 | testosterone | testosterone-D3 | 0.2-50 | y=0.0428x+0.0098 | 0.9966 | 0.07 | 0.2 | 98 |
32 | 4-androstene-3 | boldenone-D3 | 0.2-50 | y=0.642x+0.0248 | 0.9995 | 0.07 | 0.2 | 99 |
33 | prasterone | boldenone-D3 | 0.2-50 | y=0.135x+0.175 | 0.9982 | 0.07 | 0.2 | 123 |
34 | progesterone | progesterone-D9 | 0.2-50 | y=0.556x+0.0887 | 0.9983 | 0.07 | 0.2 | 89 |
35 | chlormadinone acetate | progesterone-D9 | 0.2-50 | y=0.00469x-0.0017 | 0.9987 | 0.07 | 0.2 | 127 |
36 | melengestrol acetate | progesterone-D9 | 0.2-50 | y=0.0538x+0.0016 | 0.9998 | 0.07 | 0.2 | 123 |
37 | medroxyprogesterone acetate | progesterone-D9 | 0.2-50 | y=0.0671x-0.0176 | 0.9987 | 0.07 | 0.2 | 123 |
38 | 17-α-hydroxyprogesterone | testosterone-D3 | 0.2-50 | y=0.158x-0.0587 | 0.9940 | 0.07 | 0.2 | 107 |
39 | megestrol | methyltestosterone-D3 | 0.2-50 | y=0.0298x+0.0062 | 0.9976 | 0.07 | 0.2 | 118 |
40 | triamterene | ractopamine-D5 | 0.2-50 | y=0.998x+1.474 | 0.9993 | 0.07 | 0.2 | 108 |
41 | spironolactone | boldenone-D3 | 0.2-50 | y=0.980x+0.112 | 0.9992 | 0.07 | 0.2 | 104 |
42 | canrenone | testosterone-D3 | 0.2-50 | y=0.0116x+0.0023 | 0.9972 | 0.07 | 0.2 | 99 |
43 | dexamethasone | dexamethasone-D5 | 0.5-200 | y=2.269x+0.170 | 0.9995 | 0.12 | 0.4 | 94 |
44 | hydrocortisone | hydrocortisone-D3 | 0.5-100 | y=0.630x+0.044 | 0.9991 | 0.12 | 0.4 | 99 |
45 | prednisolone | hydrocortisone-D3 | 0.5-200 | y=0.131x+0.0.038 | 0.9964 | 0.12 | 0.4 | 85 |
46 | cortisone | hydrocortisone-D3 | 0.5-100 | y=0.894x+0.056 | 0.9986 | 0.12 | 0.4 | 82 |
47 | prednisone | hydrocortisone-D3 | 0.5-100 | y=0.272x-0.00203 | 0.9996 | 0.12 | 0.4 | 91 |
48 | fluocinolone acetonide | hydrocortisone-D3 | 0.5-100 | y=0.446x+0.0587 | 0.9934 | 0.12 | 0.4 | 80 |
49 | fludrocortisone | hydrocortisone-D3 | 0.5-100 | y=0.218x-0.00661 | 0.9999 | 0.12 | 0.4 | 81 |
50 | beclomethasone | hydrocortisone-D3 | 0.5-100 | y=0.0535x+0.0115 | 0.9992 | 0.12 | 0.4 | 60 |
Table 2 Internal standards, linear ranges, linear equations, correlation coefficients (R2), limits of detection (LODs), limits of quantification (LOQs), and matrix effects (SSE) of the 50 target analytes
No. | Compound | Internal standard* | Linear range/ (μg/L) | Linear equation | R2 | LOD/ (μg/kg) | LOQ/ (μg/kg) | SSE/ % |
---|---|---|---|---|---|---|---|---|
1 | tulobuterol | clenbuterol-D9 | 0.1-20 | y=1.008x+0.0127 | 0.9992 | 0.03 | 0.1 | 109 |
2 | clenbuterol | clenbuterol-D9 | 0.1-20 | y=1.259x+0.0982 | 0.9994 | 0.03 | 0.1 | 97 |
3 | bambuterol | clenbuterol-D9 | 0.1-20 | y=0.415x-0.0548 | 0.9995 | 0.03 | 0.1 | 148 |
4 | salmeterol | ractopamine-D5 | 0.1-20 | y=0.339x-0.0420 | 0.9980 | 0.03 | 0.1 | 133 |
5 | clenproperol | clenbuterol-D9 | 0.2-20 | y=0.725x+0.0577 | 0.9992 | 0.07 | 0.2 | 108 |
6 | zilpaterol | salbutamol-D3 | 0.1-20 | y=0.921x+0.163 | 0.9975 | 0.03 | 0.1 | 85 |
7 | fenoterol | salbutamol-D3 | 0.1-20 | y=1.119x-0.0307 | 0.9992 | 0.03 | 0.1 | 104 |
8 | penbuterol | clenbuterol-D9 | 0.1-10 | y=4.360x+0.259 | 0.9961 | 0.03 | 0.1 | 129 |
9 | clencyclohexerol | clenbuterol-D9 | 0.1-20 | y=1.324x+0.132 | 0.9985 | 0.03 | 0.1 | 80 |
10 | mabuterol | clenbuterol-D9 | 0.2-20 | y=0.116x+0.00952 | 0.9991 | 0.07 | 0.2 | 108 |
11 | brombuterol | clenbuterol-D9 | 0.1-20 | y=0.137x-0.00338 | 0.9993 | 0.03 | 0.1 | 124 |
12 | cimaterol | clenbuterol-D9 | 0.2-20 | y=1.042x+0.0599 | 0.9996 | 0.07 | 0.2 | 117 |
13 | salbutamol | salbutamol-D3 | 0.1-10 | y=0.432x+0.0494 | 0.9971 | 0.03 | 0.1 | 105 |
14 | metaproterenol | clenbuterol-D9 | 0.1-20 | y=2.046x-0.0725 | 0.9993 | 0.03 | 0.1 | 103 |
15 | terbutaline | clenbuterol-D9 | 0.1-10 | y=3.548x+0.159 | 0.9987 | 0.03 | 0.1 | 138 |
16 | clorprenaline | clenbuterol-D9 | 0.1-20 | y=0.752x+0.0253 | 0.9997 | 0.03 | 0.1 | 177 |
17 | ractopamine | ractopamine-D5 | 0.1-20 | y=1.121x+0.390 | 0.9989 | 0.03 | 0.1 | 92 |
18 | demethyl coclaurine | demethyl coclaurine-D4 | 0.1-10 | y=3.200x+0.0441 | 0.9999 | 0.03 | 0.1 | 92 |
19 | tretoquinol | tretoquinol-D9 | 0.1-20 | y=0.146x-0.00404 | 0.9994 | 0.03 | 0.1 | 115 |
20 | atenolol | clenbuterol-D9 | 0.1-20 | y=1.789x+0.333 | 0.9959 | 0.03 | 0.1 | 127 |
21 | propranolol | clenbuterol-D9 | 0.1-20 | y=1.761x+0.0714 | 0.9996 | 0.03 | 0.1 | 87 |
22 | metoprolol | clenbuterol-D9 | 0.1-20 | y=1.137x+0.0171 | 0.9999 | 0.03 | 0.1 | 75 |
23 | trenbolone | boldenone-D3 | 0.2-50 | y=2.423x+1.230 | 0.9951 | 0.07 | 0.2 | 112 |
24 | methyltestosterone | methyltestosterone-D3 | 0.2-50 | y=0.737x+0.175 | 0.9957 | 0.07 | 0.2 | 90 |
25 | boldenone | boldenone-D3 | 0.2-50 | y=3.571x+0.923 | 0.9971 | 0.07 | 0.2 | 85 |
26 | nortestosterone | testosterone-D3 | 0.2-50 | y=0.0158x+0.0105 | 0.9963 | 0.07 | 0.2 | 106 |
27 | stanozolol | progesterone-D9 | 0.2-50 | y=1.858x-0.138 | 0.9987 | 0.07 | 0.2 | 103 |
28 | methandienone | testosterone-D3 | 0.2-50 | y=0.022x+0.0111 | 0.9951 | 0.07 | 0.2 | 95 |
29 | mesterolone | methyltestosterone-D3 | 0.2-50 | y=0.0284x+0.0152 | 0.9966 | 0.07 | 0.2 | 173 |
30 | mestanolone | methyltestosterone-D3 | 0.2-50 | y=0.0274x-0.0303 | 0.9957 | 0.07 | 0.2 | 95 |
31 | testosterone | testosterone-D3 | 0.2-50 | y=0.0428x+0.0098 | 0.9966 | 0.07 | 0.2 | 98 |
32 | 4-androstene-3 | boldenone-D3 | 0.2-50 | y=0.642x+0.0248 | 0.9995 | 0.07 | 0.2 | 99 |
33 | prasterone | boldenone-D3 | 0.2-50 | y=0.135x+0.175 | 0.9982 | 0.07 | 0.2 | 123 |
34 | progesterone | progesterone-D9 | 0.2-50 | y=0.556x+0.0887 | 0.9983 | 0.07 | 0.2 | 89 |
35 | chlormadinone acetate | progesterone-D9 | 0.2-50 | y=0.00469x-0.0017 | 0.9987 | 0.07 | 0.2 | 127 |
36 | melengestrol acetate | progesterone-D9 | 0.2-50 | y=0.0538x+0.0016 | 0.9998 | 0.07 | 0.2 | 123 |
37 | medroxyprogesterone acetate | progesterone-D9 | 0.2-50 | y=0.0671x-0.0176 | 0.9987 | 0.07 | 0.2 | 123 |
38 | 17-α-hydroxyprogesterone | testosterone-D3 | 0.2-50 | y=0.158x-0.0587 | 0.9940 | 0.07 | 0.2 | 107 |
39 | megestrol | methyltestosterone-D3 | 0.2-50 | y=0.0298x+0.0062 | 0.9976 | 0.07 | 0.2 | 118 |
40 | triamterene | ractopamine-D5 | 0.2-50 | y=0.998x+1.474 | 0.9993 | 0.07 | 0.2 | 108 |
41 | spironolactone | boldenone-D3 | 0.2-50 | y=0.980x+0.112 | 0.9992 | 0.07 | 0.2 | 104 |
42 | canrenone | testosterone-D3 | 0.2-50 | y=0.0116x+0.0023 | 0.9972 | 0.07 | 0.2 | 99 |
43 | dexamethasone | dexamethasone-D5 | 0.5-200 | y=2.269x+0.170 | 0.9995 | 0.12 | 0.4 | 94 |
44 | hydrocortisone | hydrocortisone-D3 | 0.5-100 | y=0.630x+0.044 | 0.9991 | 0.12 | 0.4 | 99 |
45 | prednisolone | hydrocortisone-D3 | 0.5-200 | y=0.131x+0.0.038 | 0.9964 | 0.12 | 0.4 | 85 |
46 | cortisone | hydrocortisone-D3 | 0.5-100 | y=0.894x+0.056 | 0.9986 | 0.12 | 0.4 | 82 |
47 | prednisone | hydrocortisone-D3 | 0.5-100 | y=0.272x-0.00203 | 0.9996 | 0.12 | 0.4 | 91 |
48 | fluocinolone acetonide | hydrocortisone-D3 | 0.5-100 | y=0.446x+0.0587 | 0.9934 | 0.12 | 0.4 | 80 |
49 | fludrocortisone | hydrocortisone-D3 | 0.5-100 | y=0.218x-0.00661 | 0.9999 | 0.12 | 0.4 | 81 |
50 | beclomethasone | hydrocortisone-D3 | 0.5-100 | y=0.0535x+0.0115 | 0.9992 | 0.12 | 0.4 | 60 |
No. | Compound | Matrix content/ (μg/kg) | Added levels* | ||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Low | Middle | High | |||||||||||
Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | ||||||||
1 | tulobuterol | - | 73.0 | 8.55 | 93.0 | 7.05 | 98.7 | 5.10 | |||||
2 | clenbuterol | - | 70.0 | 14.3 | 92.0 | 6.61 | 114.7 | 10.7 | |||||
3 | bambuterol | - | 77.0 | 7.90 | 93.3 | 9.66 | 106.7 | 1.08 | |||||
4 | salmeterol | - | 90.0 | 11.1 | 99.0 | 3.50 | 92.7 | 4.49 | |||||
5 | clenproperol | - | - | - | 74.3 | 3.88 | 85.3 | 1.35 | |||||
6 | zilpaterol | - | 66.7 | 8.66 | 78.3 | 8.97 | 102.0 | 8.55 | |||||
7 | fenoterol | - | 72.7 | 4.20 | 78.0 | 2.56 | 92.2 | 1.04 | |||||
8 | penbuterol | - | 65.0 | 7.69 | 80.3 | 10.1 | 93.3 | 9.90 | |||||
9 | clencyclohexerol | - | 62.3 | 4.04 | 70.7 | 10.6 | 101.3 | 10.9 | |||||
10 | mabuterol | - | - | - | 96.7 | 8.68 | 102.0 | 1.96 | |||||
11 | brombuterol | - | 83.0 | 13.6 | 94.7 | 8.07 | 92.7 | 1.25 | |||||
12 | cimaterol | - | - | - | 114.3 | 1.82 | 106.0 | 3.27 | |||||
13 | salbutamol | - | 76.7 | 7.53 | 95.0 | 7.37 | 91.0 | 1.10 | |||||
14 | metaproterenol | - | 62.0 | 5.59 | 65.0 | 4.62 | 76.0 | 0.76 | |||||
15 | terbutaline | - | 80.0 | 12.5 | 100.7 | 8.45 | 101.7 | 2.48 | |||||
16 | clorprenaline | - | 80.3 | 13.1 | 92.0 | 9.29 | 102.7 | 2.98 | |||||
17 | ractopamine | - | 83.3 | 6.93 | 94.0 | 7.45 | 108.7 | 3.83 | |||||
18 | demethyl coclaurine | - | 98.7 | 5.21 | 103.2 | 3.02 | 112.3 | 5.05 | |||||
19 | tretoquinol | - | 95.2 | 6.02 | 103.5 | 5.33 | 110.5 | 2.04 | |||||
20 | atenolol | - | 83.7 | 7.59 | 87.3 | 8.28 | 107.3 | 3.88 | |||||
21 | propranolol | - | 86.7 | 13.3 | 86.3 | 13.4 | 106.7 | 12.1 | |||||
22 | metoprolol | - | 76.7 | 15.1 | 92.0 | 9.78 | 108.7 | 5.92 | |||||
23 | trenbolone | - | 72.7 | 3.18 | 72.1 | 0.58 | 76.8 | 2.13 | |||||
24 | methyltestosterone | - | 73.3 | 1.57 | 108.1 | 5.98 | 94.6 | 2.65 | |||||
25 | boldenone | - | 79.3 | 5.25 | 100.6 | 7.75 | 96.0 | 2.60 | |||||
26 | nortestosterone | - | 112.0 | 1.79 | 113.3 | 4.08 | 105.8 | 3.15 | |||||
27 | stanozolol | 104.3 | 2.77 | 87.2 | 0.92 | 73.8 | 3.45 | ||||||
28 | methandienone | - | 104.7 | 3.98 | 103.5 | 2.30 | 105.9 | 3.21 | |||||
29 | mesterolone | - | 52.0 | 3.85 | 52.3 | 9.23 | 50.4 | 8.40 | |||||
30 | mestanolone | - | 52.3 | 7.72 | 55.4 | 10.2 | 50.3 | 10.2 | |||||
31 | testosterone | - | 84.7 | 3.61 | 89.3 | 7.71 | 97.9 | 6.14 | |||||
32 | 4-androstene-3 | - | 103.0 | 2.57 | 103.1 | 1.81 | 93.0 | 2.78 | |||||
33 | prasterone | - | 74.7 | 0.77 | 64.0 | 6.12 | 74.5 | 4.37 | |||||
34 | progesterone | 104.7 | 3.86 | 113.1 | 10.5 | 92.0 | 0.87 | ||||||
35 | chlormadinone acetate | - | 84.0 | 2.38 | 82.4 | 5.55 | 86.1 | 0.76 | |||||
36 | melengestrol acetate | - | 93.3 | 8.66 | 85.1 | 9.87 | 93.5 | 7.92 | |||||
37 | medroxyprogesterone acetate | - | 96.0 | 2.08 | 87.4 | 1.05 | 88.5 | 0.94 | |||||
38 | 17-α-hydroxyprogesterone | - | 103.3 | 5.59 | 93.3 | 6.19 | 101.3 | 6.57 | |||||
39 | megestrol | - | 88.3 | 8.65 | 63.3 | 9.12 | 73.7 | 7.84 | |||||
40 | triamterene | - | 62.7 | 4.02 | 74.4 | 9.17 | 66.0 | 9.09 | |||||
41 | spironolactone | - | 62.3 | 2.45 | 67.9 | 7.06 | 67.3 | 3.74 | |||||
42 | canrenone | - | 90.0 | 11.1 | 100.0 | 7.00 | 72.0 | 5.56 | |||||
43 | dexamethasone | - | 95.7 | 5.76 | 106.7 | 0.89 | 103.5 | 2.17 | |||||
44 | hydrocortisone | - | 112.7 | 3.36 | 88.7 | 3.17 | 97.2 | 1.52 | |||||
45 | prednisolone | - | 85.3 | 11.1 | 93.6 | 10.1 | 83.8 | 3.58 | |||||
46 | cortisone | - | 78.3 | 7.03 | 71.9 | 0.42 | 73.3 | 5.51 | |||||
47 | prednisone | - | 90.0 | 5.09 | 72.7 | 2.21 | 76.5 | 7.98 | |||||
48 | fluocinolone acetonide | - | 85.3 | 1.35 | 85.7 | 5.39 | 66.3 | 2.51 | |||||
49 | fludrocortisone | - | 91.7 | 4.92 | 80.8 | 5.74 | 62.4 | 4.49 | |||||
50 | beclomethasone | - | 70.3 | 9.16 | 68.2 | 8.69 | 72.5 | 6.69 |
Table 3 Spiked recoveries and precisions of the target compounds in a chicken sample (n=6)
No. | Compound | Matrix content/ (μg/kg) | Added levels* | ||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Low | Middle | High | |||||||||||
Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | ||||||||
1 | tulobuterol | - | 73.0 | 8.55 | 93.0 | 7.05 | 98.7 | 5.10 | |||||
2 | clenbuterol | - | 70.0 | 14.3 | 92.0 | 6.61 | 114.7 | 10.7 | |||||
3 | bambuterol | - | 77.0 | 7.90 | 93.3 | 9.66 | 106.7 | 1.08 | |||||
4 | salmeterol | - | 90.0 | 11.1 | 99.0 | 3.50 | 92.7 | 4.49 | |||||
5 | clenproperol | - | - | - | 74.3 | 3.88 | 85.3 | 1.35 | |||||
6 | zilpaterol | - | 66.7 | 8.66 | 78.3 | 8.97 | 102.0 | 8.55 | |||||
7 | fenoterol | - | 72.7 | 4.20 | 78.0 | 2.56 | 92.2 | 1.04 | |||||
8 | penbuterol | - | 65.0 | 7.69 | 80.3 | 10.1 | 93.3 | 9.90 | |||||
9 | clencyclohexerol | - | 62.3 | 4.04 | 70.7 | 10.6 | 101.3 | 10.9 | |||||
10 | mabuterol | - | - | - | 96.7 | 8.68 | 102.0 | 1.96 | |||||
11 | brombuterol | - | 83.0 | 13.6 | 94.7 | 8.07 | 92.7 | 1.25 | |||||
12 | cimaterol | - | - | - | 114.3 | 1.82 | 106.0 | 3.27 | |||||
13 | salbutamol | - | 76.7 | 7.53 | 95.0 | 7.37 | 91.0 | 1.10 | |||||
14 | metaproterenol | - | 62.0 | 5.59 | 65.0 | 4.62 | 76.0 | 0.76 | |||||
15 | terbutaline | - | 80.0 | 12.5 | 100.7 | 8.45 | 101.7 | 2.48 | |||||
16 | clorprenaline | - | 80.3 | 13.1 | 92.0 | 9.29 | 102.7 | 2.98 | |||||
17 | ractopamine | - | 83.3 | 6.93 | 94.0 | 7.45 | 108.7 | 3.83 | |||||
18 | demethyl coclaurine | - | 98.7 | 5.21 | 103.2 | 3.02 | 112.3 | 5.05 | |||||
19 | tretoquinol | - | 95.2 | 6.02 | 103.5 | 5.33 | 110.5 | 2.04 | |||||
20 | atenolol | - | 83.7 | 7.59 | 87.3 | 8.28 | 107.3 | 3.88 | |||||
21 | propranolol | - | 86.7 | 13.3 | 86.3 | 13.4 | 106.7 | 12.1 | |||||
22 | metoprolol | - | 76.7 | 15.1 | 92.0 | 9.78 | 108.7 | 5.92 | |||||
23 | trenbolone | - | 72.7 | 3.18 | 72.1 | 0.58 | 76.8 | 2.13 | |||||
24 | methyltestosterone | - | 73.3 | 1.57 | 108.1 | 5.98 | 94.6 | 2.65 | |||||
25 | boldenone | - | 79.3 | 5.25 | 100.6 | 7.75 | 96.0 | 2.60 | |||||
26 | nortestosterone | - | 112.0 | 1.79 | 113.3 | 4.08 | 105.8 | 3.15 | |||||
27 | stanozolol | 104.3 | 2.77 | 87.2 | 0.92 | 73.8 | 3.45 | ||||||
28 | methandienone | - | 104.7 | 3.98 | 103.5 | 2.30 | 105.9 | 3.21 | |||||
29 | mesterolone | - | 52.0 | 3.85 | 52.3 | 9.23 | 50.4 | 8.40 | |||||
30 | mestanolone | - | 52.3 | 7.72 | 55.4 | 10.2 | 50.3 | 10.2 | |||||
31 | testosterone | - | 84.7 | 3.61 | 89.3 | 7.71 | 97.9 | 6.14 | |||||
32 | 4-androstene-3 | - | 103.0 | 2.57 | 103.1 | 1.81 | 93.0 | 2.78 | |||||
33 | prasterone | - | 74.7 | 0.77 | 64.0 | 6.12 | 74.5 | 4.37 | |||||
34 | progesterone | 104.7 | 3.86 | 113.1 | 10.5 | 92.0 | 0.87 | ||||||
35 | chlormadinone acetate | - | 84.0 | 2.38 | 82.4 | 5.55 | 86.1 | 0.76 | |||||
36 | melengestrol acetate | - | 93.3 | 8.66 | 85.1 | 9.87 | 93.5 | 7.92 | |||||
37 | medroxyprogesterone acetate | - | 96.0 | 2.08 | 87.4 | 1.05 | 88.5 | 0.94 | |||||
38 | 17-α-hydroxyprogesterone | - | 103.3 | 5.59 | 93.3 | 6.19 | 101.3 | 6.57 | |||||
39 | megestrol | - | 88.3 | 8.65 | 63.3 | 9.12 | 73.7 | 7.84 | |||||
40 | triamterene | - | 62.7 | 4.02 | 74.4 | 9.17 | 66.0 | 9.09 | |||||
41 | spironolactone | - | 62.3 | 2.45 | 67.9 | 7.06 | 67.3 | 3.74 | |||||
42 | canrenone | - | 90.0 | 11.1 | 100.0 | 7.00 | 72.0 | 5.56 | |||||
43 | dexamethasone | - | 95.7 | 5.76 | 106.7 | 0.89 | 103.5 | 2.17 | |||||
44 | hydrocortisone | - | 112.7 | 3.36 | 88.7 | 3.17 | 97.2 | 1.52 | |||||
45 | prednisolone | - | 85.3 | 11.1 | 93.6 | 10.1 | 83.8 | 3.58 | |||||
46 | cortisone | - | 78.3 | 7.03 | 71.9 | 0.42 | 73.3 | 5.51 | |||||
47 | prednisone | - | 90.0 | 5.09 | 72.7 | 2.21 | 76.5 | 7.98 | |||||
48 | fluocinolone acetonide | - | 85.3 | 1.35 | 85.7 | 5.39 | 66.3 | 2.51 | |||||
49 | fludrocortisone | - | 91.7 | 4.92 | 80.8 | 5.74 | 62.4 | 4.49 | |||||
50 | beclomethasone | - | 70.3 | 9.16 | 68.2 | 8.69 | 72.5 | 6.69 |
No. | Compound | Matrix content/ (μg/kg) | Added levels* | ||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Low | Middle | High | |||||||||||
Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | ||||||||
1 | tulobuterol | - | 93.3 | 6.19 | 100.3 | 0.58 | 105.7 | 3.82 | |||||
2 | clenbuterol | - | 92.0 | 7.84 | 105.0 | 4.36 | 110.7 | 5.52 | |||||
3 | bambuterol | - | 92.0 | 3.77 | 92.0 | 6.79 | 104.0 | 1.92 | |||||
4 | salmeterol | - | 92.7 | 5.10 | 90.7 | 3.37 | 95.3 | 1.21 | |||||
5 | clenproperol | - | - | - | 116.3 | 2.76 | 107.3 | 3.53 | |||||
6 | zilpaterol | - | 84.7 | 3.61 | 100.0 | 10.0 | 103.3 | 4.03 | |||||
7 | fenoterol | - | 97.8 | 1.97 | 72.2 | 9.61 | 84.4 | 12.8 | |||||
8 | penbuterol | - | 85.3 | 2.95 | 87.7 | 7.76 | 110.0 | 6.56 | |||||
9 | clencyclohexerol | - | 93.7 | 5.05 | 92.7 | 4.98 | 108.7 | 6.46 | |||||
10 | mabuterol | - | - | - | 97.7 | 11.0 | 85.0 | 5.13 | |||||
11 | brombuterol | - | 87.0 | 6.99 | 81.3 | 1.88 | 86.0 | 2.33 | |||||
12 | cimaterol | - | - | - | 107.3 | 4.30 | 112.7 | 4.19 | |||||
13 | salbutamol | - | 93.3 | 4.83 | 110.7 | 8.15 | 114.0 | 1.75 | |||||
14 | metaproterenol | - | 107.0 | 4.07 | 99.7 | 10.0 | 112.0 | 3.57 | |||||
15 | terbutaline | - | 110.3 | 2.09 | 91.0 | 8.30 | 86.7 | 2.90 | |||||
16 | clorprenaline | - | 100.0 | 1.34 | 110.0 | 1.76 | 111.3 | 4.52 | |||||
17 | ractopamine | - | 75.3 | 5.03 | 66.7 | 8.66 | 62.7 | 9.75 | |||||
18 | demethyl coclaurine | - | 95.3 | 4.73 | 105.7 | 2.73 | 110.7 | 3.09 | |||||
19 | tretoquinol | - | 84.0 | 4.76 | 89.3 | 7.28 | 93.7 | 5.88 | |||||
20 | atenolol | - | 96.0 | 5.51 | 110.0 | 1.69 | 110.7 | 2.09 | |||||
21 | propranolol | - | 98.8 | 6.21 | 97.5 | 5.28 | 106.3 | 3.32 | |||||
22 | metoprolol | - | 95.1 | 4.02 | 97.6 | 5.33 | 113.2 | 5.71 | |||||
21 | trenbolone | - | 76.7 | 7.53 | 77.3 | 1.49 | 77.6 | 3.57 | |||||
24 | methyltestosterone | - | 97.8 | 1.97 | 98.7 | 7.67 | 105.3 | 2.32 | |||||
25 | boldenone | - | 113.3 | 10.2 | 102.7 | 2.98 | 104.0 | 4.62 | |||||
26 | nortestosterone | - | 114.0 | 3.04 | 113.4 | 3.12 | 115.8 | 2.88 | |||||
27 | stanozolol | - | 65.3 | 7.70 | 66.7 | 4.58 | 70.8 | 10.6 | |||||
28 | methandienone | - | 103.3 | 5.59 | 100.7 | 4.14 | 105.9 | 3.21 | |||||
29 | mesterolone | - | 51.0 | 7.07 | 51.3 | 5.95 | 50.4 | 8.40 | |||||
30 | mestanolone | - | 50.3 | 3.03 | 53.7 | 9.19 | 57.7 | 4.36 | |||||
31 | testosterone | - | 75.0 | 6.67 | 103.3 | 1.12 | 97.9 | 6.14 | |||||
32 | 4-androstene-3 | - | 113.3 | 5.09 | 113.0 | 3.86 | 99.1 | 4.45 | |||||
33 | prasterone | - | 61.3 | 3.77 | 64.0 | 4.13 | 66.3 | 4.61 | |||||
34 | progesterone | - | 93.3 | 12.4 | 98.7 | 6.59 | 92.0 | 0.87 | |||||
35 | chlormadinone acetate | - | 70.0 | 4.01 | 69.7 | 3.61 | 66.1 | 0.99 | |||||
36 | melengestrol acetate | - | 96.7 | 5.97 | 84.0 | 12.6 | 83.5 | 10.9 | |||||
37 | medroxyprogesterone acetate | - | 68.3 | 11.2 | 72.7 | 4.20 | 78.5 | 1.06 | |||||
38 | 17-α-hydroxyprogesterone | - | 79.0 | 8.86 | 69.4 | 9.32 | 74.6 | 7.34 | |||||
39 | megestrol | - | 70.3 | 7.83 | 69.3 | 7.08 | 87.4 | 5.15 | |||||
40 | triamterene | - | 65.0 | 10.8 | 65.0 | 7.69 | 66.0 | 9.09 | |||||
41 | spironolactone | - | 69.3 | 1.67 | 72.0 | 8.45 | 74.0 | 7.15 | |||||
42 | canrenone | - | 100.0 | 5.04 | 73.3 | 7.87 | 72.0 | 5.56 | |||||
43 | dexamethasone | - | 116.7 | 4.95 | 105.7 | 3.04 | 78.9 | 4.79 | |||||
44 | hydrocortisone | 13.3 | 87.3 | 7.36 | 105.7 | 5.21 | 70.8 | 9.09 | |||||
45 | prednisolone | - | 60.0 | 5.96 | 73.3 | 9.86 | 63.6 | 4.75 | |||||
46 | cortisone | 3.86 | 62.0 | 8.06 | 96.4 | 7.86 | 73.1 | 5.92 | |||||
47 | prednisone | - | 66.0 | 8.44 | 74.3 | 7.41 | 76.5 | 7.98 | |||||
48 | fluocinolone acetonide | - | 65.3 | 6.37 | 82.0 | 6.34 | 66.3 | 2.51 | |||||
49 | fludrocortisone | - | 87.3 | 7.36 | 87.3 | 11.6 | 62.4 | 4.49 | |||||
50 | beclomethasone | - | 77.6 | 10.3 | 81.1 | 1.05 | 69.1 | 6.41 |
Table 4 Spiked recoveries and precisions of the target compounds in a pork sample (n=6)
No. | Compound | Matrix content/ (μg/kg) | Added levels* | ||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Low | Middle | High | |||||||||||
Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | ||||||||
1 | tulobuterol | - | 93.3 | 6.19 | 100.3 | 0.58 | 105.7 | 3.82 | |||||
2 | clenbuterol | - | 92.0 | 7.84 | 105.0 | 4.36 | 110.7 | 5.52 | |||||
3 | bambuterol | - | 92.0 | 3.77 | 92.0 | 6.79 | 104.0 | 1.92 | |||||
4 | salmeterol | - | 92.7 | 5.10 | 90.7 | 3.37 | 95.3 | 1.21 | |||||
5 | clenproperol | - | - | - | 116.3 | 2.76 | 107.3 | 3.53 | |||||
6 | zilpaterol | - | 84.7 | 3.61 | 100.0 | 10.0 | 103.3 | 4.03 | |||||
7 | fenoterol | - | 97.8 | 1.97 | 72.2 | 9.61 | 84.4 | 12.8 | |||||
8 | penbuterol | - | 85.3 | 2.95 | 87.7 | 7.76 | 110.0 | 6.56 | |||||
9 | clencyclohexerol | - | 93.7 | 5.05 | 92.7 | 4.98 | 108.7 | 6.46 | |||||
10 | mabuterol | - | - | - | 97.7 | 11.0 | 85.0 | 5.13 | |||||
11 | brombuterol | - | 87.0 | 6.99 | 81.3 | 1.88 | 86.0 | 2.33 | |||||
12 | cimaterol | - | - | - | 107.3 | 4.30 | 112.7 | 4.19 | |||||
13 | salbutamol | - | 93.3 | 4.83 | 110.7 | 8.15 | 114.0 | 1.75 | |||||
14 | metaproterenol | - | 107.0 | 4.07 | 99.7 | 10.0 | 112.0 | 3.57 | |||||
15 | terbutaline | - | 110.3 | 2.09 | 91.0 | 8.30 | 86.7 | 2.90 | |||||
16 | clorprenaline | - | 100.0 | 1.34 | 110.0 | 1.76 | 111.3 | 4.52 | |||||
17 | ractopamine | - | 75.3 | 5.03 | 66.7 | 8.66 | 62.7 | 9.75 | |||||
18 | demethyl coclaurine | - | 95.3 | 4.73 | 105.7 | 2.73 | 110.7 | 3.09 | |||||
19 | tretoquinol | - | 84.0 | 4.76 | 89.3 | 7.28 | 93.7 | 5.88 | |||||
20 | atenolol | - | 96.0 | 5.51 | 110.0 | 1.69 | 110.7 | 2.09 | |||||
21 | propranolol | - | 98.8 | 6.21 | 97.5 | 5.28 | 106.3 | 3.32 | |||||
22 | metoprolol | - | 95.1 | 4.02 | 97.6 | 5.33 | 113.2 | 5.71 | |||||
21 | trenbolone | - | 76.7 | 7.53 | 77.3 | 1.49 | 77.6 | 3.57 | |||||
24 | methyltestosterone | - | 97.8 | 1.97 | 98.7 | 7.67 | 105.3 | 2.32 | |||||
25 | boldenone | - | 113.3 | 10.2 | 102.7 | 2.98 | 104.0 | 4.62 | |||||
26 | nortestosterone | - | 114.0 | 3.04 | 113.4 | 3.12 | 115.8 | 2.88 | |||||
27 | stanozolol | - | 65.3 | 7.70 | 66.7 | 4.58 | 70.8 | 10.6 | |||||
28 | methandienone | - | 103.3 | 5.59 | 100.7 | 4.14 | 105.9 | 3.21 | |||||
29 | mesterolone | - | 51.0 | 7.07 | 51.3 | 5.95 | 50.4 | 8.40 | |||||
30 | mestanolone | - | 50.3 | 3.03 | 53.7 | 9.19 | 57.7 | 4.36 | |||||
31 | testosterone | - | 75.0 | 6.67 | 103.3 | 1.12 | 97.9 | 6.14 | |||||
32 | 4-androstene-3 | - | 113.3 | 5.09 | 113.0 | 3.86 | 99.1 | 4.45 | |||||
33 | prasterone | - | 61.3 | 3.77 | 64.0 | 4.13 | 66.3 | 4.61 | |||||
34 | progesterone | - | 93.3 | 12.4 | 98.7 | 6.59 | 92.0 | 0.87 | |||||
35 | chlormadinone acetate | - | 70.0 | 4.01 | 69.7 | 3.61 | 66.1 | 0.99 | |||||
36 | melengestrol acetate | - | 96.7 | 5.97 | 84.0 | 12.6 | 83.5 | 10.9 | |||||
37 | medroxyprogesterone acetate | - | 68.3 | 11.2 | 72.7 | 4.20 | 78.5 | 1.06 | |||||
38 | 17-α-hydroxyprogesterone | - | 79.0 | 8.86 | 69.4 | 9.32 | 74.6 | 7.34 | |||||
39 | megestrol | - | 70.3 | 7.83 | 69.3 | 7.08 | 87.4 | 5.15 | |||||
40 | triamterene | - | 65.0 | 10.8 | 65.0 | 7.69 | 66.0 | 9.09 | |||||
41 | spironolactone | - | 69.3 | 1.67 | 72.0 | 8.45 | 74.0 | 7.15 | |||||
42 | canrenone | - | 100.0 | 5.04 | 73.3 | 7.87 | 72.0 | 5.56 | |||||
43 | dexamethasone | - | 116.7 | 4.95 | 105.7 | 3.04 | 78.9 | 4.79 | |||||
44 | hydrocortisone | 13.3 | 87.3 | 7.36 | 105.7 | 5.21 | 70.8 | 9.09 | |||||
45 | prednisolone | - | 60.0 | 5.96 | 73.3 | 9.86 | 63.6 | 4.75 | |||||
46 | cortisone | 3.86 | 62.0 | 8.06 | 96.4 | 7.86 | 73.1 | 5.92 | |||||
47 | prednisone | - | 66.0 | 8.44 | 74.3 | 7.41 | 76.5 | 7.98 | |||||
48 | fluocinolone acetonide | - | 65.3 | 6.37 | 82.0 | 6.34 | 66.3 | 2.51 | |||||
49 | fludrocortisone | - | 87.3 | 7.36 | 87.3 | 11.6 | 62.4 | 4.49 | |||||
50 | beclomethasone | - | 77.6 | 10.3 | 81.1 | 1.05 | 69.1 | 6.41 |
No. | Compound | Matrix content/ (μg/kg) | Added levels* | ||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Low | Middle | High | |||||||||||
Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | ||||||||
1 | tulobuterol | - | 111.0 | 0.90 | 104.3 | 2.21 | 102.8 | 1.08 | |||||
2 | clenbuterol | - | 116.0 | 3.95 | 95.0 | 3.80 | 107.8 | 9.55 | |||||
3 | bambuterol | - | 105.0 | 5.79 | 113.0 | 4.06 | 104.7 | 6.25 | |||||
4 | salmeterol | - | 102.7 | 14.6 | 70.3 | 0.82 | 80.1 | 2.31 | |||||
5 | clenproperol | - | - | - | 66.0 | 3.03 | 72.7 | 5.39 | |||||
6 | zilpaterol | - | 110.0 | 4.72 | 65.3 | 9.96 | 74.0 | 14.2 | |||||
7 | fenoterol | - | 65.6 | 10.6 | 66.7 | 4.58 | 76.1 | 4.99 | |||||
8 | penbuterol | - | 114.3 | 0.50 | 76.7 | 2.72 | 70.0 | 13.1 | |||||
9 | clencyclohexerol | - | 104.0 | 10.7 | 67.3 | 10.1 | 77.3 | 13.6 | |||||
10 | mabuterol | - | - | - | 110.0 | 7.10 | 111.8 | 9.30 | |||||
11 | brombuterol | - | 115.7 | 2.78 | 99.0 | 12.7 | 103.5 | 8.40 | |||||
12 | cimaterol | - | - | - | 98.0 | 12.8 | 96.7 | 10.0 | |||||
13 | salbutamol | - | 110.7 | 4.46 | 77.3 | 13.2 | 68.9 | 10.1 | |||||
14 | metaproterenol | - | 100.7 | 4.90 | 85.7 | 7.13 | 87.5 | 8.66 | |||||
15 | terbutaline | - | 96.0 | 1.04 | 104.3 | 11.4 | 112.7 | 6.96 | |||||
16 | clorprenaline | - | 101.0 | 0.99 | 116.0 | 2.28 | 113.7 | 2.38 | |||||
17 | ractopamine | - | 74.3 | 2.05 | 77.3 | 2.69 | 82.3 | 3.00 | |||||
18 | demethyl coclaurine | - | 84.0 | 1.19 | 85.3 | 2.95 | 79.3 | 4.68 | |||||
19 | tretoquinol | - | 94.0 | 1.06 | 102.7 | 2.98 | 104.5 | 2.15 | |||||
20 | atenolol | - | 82.7 | 2.52 | 90.0 | 2.22 | 98.9 | 11.1 | |||||
21 | propranolol | - | 96.0 | 5.38 | 101.4 | 5.08 | 105.6 | 4.03 | |||||
22 | metoprolol | - | 102.5 | 4.99 | 107.3 | 5.07 | 112.5 | 3.22 | |||||
23 | trenbolone | - | 69.3 | 4.41 | 79.7 | 10.5 | 84.3 | 11.3 | |||||
24 | methyltestosterone | - | 108.7 | 3.83 | 101.6 | 2.86 | 107.9 | 13.3 | |||||
25 | boldenone | - | 98.0 | 5.40 | 108.8 | 4.69 | 108.1 | 2.57 | |||||
26 | nortestosterone | - | 113.3 | 1.02 | 107.8 | 2.45 | 107.1 | 1.77 | |||||
27 | stanozolol | - | 70.7 | 9.94 | 55.1 | 4.67 | 55.9 | 8.23 | |||||
28 | methandienone | - | 84.7 | 5.94 | 106.7 | 3.56 | 106.4 | 7.73 | |||||
29 | mesterolone | - | 54.0 | 6.42 | 54.4 | 6.07 | 55.1 | 5.29 | |||||
30 | mestanolone | - | 60.3 | 11.0 | 54.3 | 6.08 | 52.0 | 5.75 | |||||
31 | testosterone | 1.00 | 116.7 | 3.96 | 100.4 | 2.74 | 86.3 | 12.7 | |||||
32 | 4-androstene-3 | - | 114.7 | 5.81 | 91.3 | 7.29 | 94.9 | 3.58 | |||||
33 | prasterone | - | 89.0 | 9.20 | 64.2 | 13.9 | 80.6 | 12.6 | |||||
34 | progesterone | - | 96.3 | 7.79 | 80.3 | 3.61 | 81.0 | 13.8 | |||||
35 | chlormadinone acetate | - | 67.5 | 10.1 | 80.1 | 7.22 | 81.6 | 2.62 | |||||
36 | melengestrol acetate | - | 78.8 | 2.01 | 78.5 | 1.93 | 80.4 | 9.68 | |||||
37 | medroxyprogesterone acetate | - | 64.5 | 5.74 | 119.2 | 3.35 | 113.8 | 2.14 | |||||
38 | 17-α-hydroxyprogesterone | 74.6 | 7.34 | 119.9 | 4.83 | 115.3 | 2.92 | ||||||
39 | megestrol | 87.4 | 5.15 | 66.8 | 10.6 | 66.5 | 10.8 | ||||||
40 | triamterene | - | 67.3 | 6.18 | 61.2 | 5.89 | 72.1 | 12.0 | |||||
41 | spironolactone | - | 79.9 | 5.95 | 78.5 | 8.60 | 78.7 | 8.30 | |||||
42 | canrenone | - | 71.0 | 2.82 | 105.7 | 2.38 | 105.5 | 11.2 | |||||
43 | dexamethasone | - | 99.0 | 15.0 | 105.9 | 7.60 | 104.8 | 2.75 | |||||
44 | hydrocortisone | 4.90 | 118.3 | 4.34 | 90.8 | 4.98 | 71.4 | 0.87 | |||||
45 | prednisolone | - | 62.3 | 7.58 | 78.5 | 1.75 | 75.5 | 5.53 | |||||
46 | cortisone | 1.10 | 89.0 | 4.05 | 80.5 | 6.29 | 69.7 | 5.22 | |||||
47 | prednisone | - | 86.7 | 6.56 | 72.3 | 9.10 | 77.3 | 3.42 | |||||
48 | fluocinolone acetonide | - | 63.0 | 11.4 | 84.9 | 2.35 | 69.3 | 10.7 | |||||
49 | fludrocortisone | - | 65.7 | 0.88 | 86.0 | 1.71 | 63.2 | 7.14 | |||||
50 | beclomethasone | - | 74.2 | 6.77 | 82.4 | 4.98 | 69.0 | 4.07 |
Table 5 Spiked recoveries and precisions of the target compounds in a lamb sample (n=6)
No. | Compound | Matrix content/ (μg/kg) | Added levels* | ||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Low | Middle | High | |||||||||||
Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | ||||||||
1 | tulobuterol | - | 111.0 | 0.90 | 104.3 | 2.21 | 102.8 | 1.08 | |||||
2 | clenbuterol | - | 116.0 | 3.95 | 95.0 | 3.80 | 107.8 | 9.55 | |||||
3 | bambuterol | - | 105.0 | 5.79 | 113.0 | 4.06 | 104.7 | 6.25 | |||||
4 | salmeterol | - | 102.7 | 14.6 | 70.3 | 0.82 | 80.1 | 2.31 | |||||
5 | clenproperol | - | - | - | 66.0 | 3.03 | 72.7 | 5.39 | |||||
6 | zilpaterol | - | 110.0 | 4.72 | 65.3 | 9.96 | 74.0 | 14.2 | |||||
7 | fenoterol | - | 65.6 | 10.6 | 66.7 | 4.58 | 76.1 | 4.99 | |||||
8 | penbuterol | - | 114.3 | 0.50 | 76.7 | 2.72 | 70.0 | 13.1 | |||||
9 | clencyclohexerol | - | 104.0 | 10.7 | 67.3 | 10.1 | 77.3 | 13.6 | |||||
10 | mabuterol | - | - | - | 110.0 | 7.10 | 111.8 | 9.30 | |||||
11 | brombuterol | - | 115.7 | 2.78 | 99.0 | 12.7 | 103.5 | 8.40 | |||||
12 | cimaterol | - | - | - | 98.0 | 12.8 | 96.7 | 10.0 | |||||
13 | salbutamol | - | 110.7 | 4.46 | 77.3 | 13.2 | 68.9 | 10.1 | |||||
14 | metaproterenol | - | 100.7 | 4.90 | 85.7 | 7.13 | 87.5 | 8.66 | |||||
15 | terbutaline | - | 96.0 | 1.04 | 104.3 | 11.4 | 112.7 | 6.96 | |||||
16 | clorprenaline | - | 101.0 | 0.99 | 116.0 | 2.28 | 113.7 | 2.38 | |||||
17 | ractopamine | - | 74.3 | 2.05 | 77.3 | 2.69 | 82.3 | 3.00 | |||||
18 | demethyl coclaurine | - | 84.0 | 1.19 | 85.3 | 2.95 | 79.3 | 4.68 | |||||
19 | tretoquinol | - | 94.0 | 1.06 | 102.7 | 2.98 | 104.5 | 2.15 | |||||
20 | atenolol | - | 82.7 | 2.52 | 90.0 | 2.22 | 98.9 | 11.1 | |||||
21 | propranolol | - | 96.0 | 5.38 | 101.4 | 5.08 | 105.6 | 4.03 | |||||
22 | metoprolol | - | 102.5 | 4.99 | 107.3 | 5.07 | 112.5 | 3.22 | |||||
23 | trenbolone | - | 69.3 | 4.41 | 79.7 | 10.5 | 84.3 | 11.3 | |||||
24 | methyltestosterone | - | 108.7 | 3.83 | 101.6 | 2.86 | 107.9 | 13.3 | |||||
25 | boldenone | - | 98.0 | 5.40 | 108.8 | 4.69 | 108.1 | 2.57 | |||||
26 | nortestosterone | - | 113.3 | 1.02 | 107.8 | 2.45 | 107.1 | 1.77 | |||||
27 | stanozolol | - | 70.7 | 9.94 | 55.1 | 4.67 | 55.9 | 8.23 | |||||
28 | methandienone | - | 84.7 | 5.94 | 106.7 | 3.56 | 106.4 | 7.73 | |||||
29 | mesterolone | - | 54.0 | 6.42 | 54.4 | 6.07 | 55.1 | 5.29 | |||||
30 | mestanolone | - | 60.3 | 11.0 | 54.3 | 6.08 | 52.0 | 5.75 | |||||
31 | testosterone | 1.00 | 116.7 | 3.96 | 100.4 | 2.74 | 86.3 | 12.7 | |||||
32 | 4-androstene-3 | - | 114.7 | 5.81 | 91.3 | 7.29 | 94.9 | 3.58 | |||||
33 | prasterone | - | 89.0 | 9.20 | 64.2 | 13.9 | 80.6 | 12.6 | |||||
34 | progesterone | - | 96.3 | 7.79 | 80.3 | 3.61 | 81.0 | 13.8 | |||||
35 | chlormadinone acetate | - | 67.5 | 10.1 | 80.1 | 7.22 | 81.6 | 2.62 | |||||
36 | melengestrol acetate | - | 78.8 | 2.01 | 78.5 | 1.93 | 80.4 | 9.68 | |||||
37 | medroxyprogesterone acetate | - | 64.5 | 5.74 | 119.2 | 3.35 | 113.8 | 2.14 | |||||
38 | 17-α-hydroxyprogesterone | 74.6 | 7.34 | 119.9 | 4.83 | 115.3 | 2.92 | ||||||
39 | megestrol | 87.4 | 5.15 | 66.8 | 10.6 | 66.5 | 10.8 | ||||||
40 | triamterene | - | 67.3 | 6.18 | 61.2 | 5.89 | 72.1 | 12.0 | |||||
41 | spironolactone | - | 79.9 | 5.95 | 78.5 | 8.60 | 78.7 | 8.30 | |||||
42 | canrenone | - | 71.0 | 2.82 | 105.7 | 2.38 | 105.5 | 11.2 | |||||
43 | dexamethasone | - | 99.0 | 15.0 | 105.9 | 7.60 | 104.8 | 2.75 | |||||
44 | hydrocortisone | 4.90 | 118.3 | 4.34 | 90.8 | 4.98 | 71.4 | 0.87 | |||||
45 | prednisolone | - | 62.3 | 7.58 | 78.5 | 1.75 | 75.5 | 5.53 | |||||
46 | cortisone | 1.10 | 89.0 | 4.05 | 80.5 | 6.29 | 69.7 | 5.22 | |||||
47 | prednisone | - | 86.7 | 6.56 | 72.3 | 9.10 | 77.3 | 3.42 | |||||
48 | fluocinolone acetonide | - | 63.0 | 11.4 | 84.9 | 2.35 | 69.3 | 10.7 | |||||
49 | fludrocortisone | - | 65.7 | 0.88 | 86.0 | 1.71 | 63.2 | 7.14 | |||||
50 | beclomethasone | - | 74.2 | 6.77 | 82.4 | 4.98 | 69.0 | 4.07 |
No. | Compound | Matrix content/ (μg/kg) | Added levels* | ||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Low | Middle | High | |||||||||||
Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | ||||||||
1 | tulobuterol | - | 102.3 | 2.26 | 105.3 | 3.09 | 89.9 | 5.33 | |||||
2 | clenbuterol | - | 113.7 | 2.83 | 111.5 | 7.83 | 113.9 | 5.31 | |||||
3 | bambuterol | - | 106.0 | 2.50 | 104.7 | 3.79 | 89.3 | 4.77 | |||||
4 | salmeterol | - | 87.7 | 2.37 | 98.6 | 3.03 | 97.3 | 13.2 | |||||
5 | clenproperol | - | 85.7 | 1.35 | 85.1 | 1.49 | 86.8 | 4.38 | |||||
6 | zilpaterol | - | 101.3 | 1.51 | 97.9 | 1.59 | 89.6 | 0.76 | |||||
7 | fenoterol | - | 72.0 | 2.78 | 80.9 | 4.59 | 73.9 | 5.34 | |||||
8 | penbuterol | - | 104.0 | 3.47 | 113.5 | 2.91 | 109.5 | 8.45 | |||||
9 | clencyclohexerol | - | 65.0 | 2.66 | 66.6 | 8.46 | 66.6 | 4.78 | |||||
10 | mabuterol | - | 107.7 | 3.75 | 117.7 | 1.44 | 110.3 | 0.82 | |||||
11 | brombuterol | - | 103.0 | 0.97 | 104.8 | 2.98 | 107.1 | 2.68 | |||||
12 | cimaterol | - | 112.3 | 4.39 | 103.9 | 0.99 | 105.6 | 2.18 | |||||
13 | salbutamol | - | 94.3 | 11.7 | 106.1 | 8.12 | 109.0 | 2.70 | |||||
14 | metaproterenol | - | 67.0 | 8.31 | 84.2 | 4.91 | 84.2 | 2.38 | |||||
15 | terbutaline | - | 95.0 | 5.26 | 102.3 | 8.64 | 97.5 | 10.3 | |||||
16 | clorprenaline | - | 85.0 | 4.71 | 87.9 | 1.25 | 85.0 | 1.19 | |||||
17 | ractopamine | - | 101.0 | 0.99 | 86.2 | 4.96 | 87.1 | 2.52 | |||||
18 | demethyl coclaurine | - | 93.7 | 2.47 | 88.9 | 3.64 | 89.7 | 2.77 | |||||
19 | tretoquinol | - | 84.3 | 3.81 | 84.1 | 1.80 | 87.0 | 1.59 | |||||
20 | atenolol | - | 101.0 | 3.43 | 110.2 | 6.72 | 104.5 | 3.78 | |||||
21 | propranolol | - | 92.6 | 4.52 | 99.8 | 7.01 | 100.6 | 5.01 | |||||
22 | metoprolol | - | 96.6 | 8.75 | 110.5 | 4.22 | 112.9 | 4.47 | |||||
23 | trenbolone | - | 92.3 | 5.20 | 102.7 | 2.97 | 91.9 | 1.78 | |||||
24 | methyltestosterone | - | 107.5 | 6.51 | 111.8 | 4.19 | 74.8 | 2.79 | |||||
25 | boldenone | - | 105.3 | 5.16 | 116.5 | 4.41 | 96.0 | 2.10 | |||||
26 | nortestosterone | - | 86.9 | 8.31 | 90.9 | 4.19 | 78.8 | 2.64 | |||||
27 | stanozolol | - | 51.7 | 5.58 | 54.4 | 2.57 | 52.5 | 3.25 | |||||
28 | methandienone | - | 84.3 | 4.87 | 99.1 | 3.07 | 69.0 | 3.72 | |||||
29 | mesterolone | - | 57.3 | 4.01 | 50.4 | 5.34 | 53.9 | 3.18 | |||||
30 | mestanolone | - | 53.1 | 5.50 | 52.4 | 5.86 | 53.9 | 3.36 | |||||
31 | testosterone | - | 70.1 | 5.44 | 65.8 | 7.24 | 66.0 | 1.60 | |||||
32 | 4-androstene-3 | - | 92.3 | 8.40 | 80.6 | 7.89 | 79.1 | 0.77 | |||||
33 | prasterone | - | 92.2 | 5.92 | 101.2 | 7.18 | 107.5 | 2.18 | |||||
34 | progesterone | 12.0 | 104.6 | 1.99 | 96.6 | 1.47 | 93.0 | 3.22 | |||||
35 | chlormadinone acetate | - | 63.7 | 7.66 | 75.3 | 5.81 | 68.3 | 9.47 | |||||
36 | melengestrol acetate | - | 85.3 | 12.8 | 83.4 | 12.6 | 83.7 | 8.31 | |||||
37 | medroxyprogesterone acetate | - | 90.0 | 7.95 | 93.9 | 3.31 | 97.4 | 3.41 | |||||
38 | 17-α-hydroxyprogesterone | - | 73.4 | 8.58 | 76.1 | 10.1 | 72.2 | 5.32 | |||||
39 | megestrol | - | 60.7 | 8.30 | 71.0 | 4.09 | 74.7 | 3.09 | |||||
40 | triamterene | - | 63.7 | 6.27 | 61.1 | 1.36 | 68.0 | 2.15 | |||||
41 | spironolactone | - | 91.4 | 7.03 | 83.7 | 1.97 | 86.2 | 5.03 | |||||
42 | canrenone | - | 67.3 | 5.22 | 69.1 | 3.95 | 66.5 | 2.90 | |||||
43 | dexamethasone | - | 81.2 | 7.10 | 107.8 | 3.03 | 101.2 | 10.1 | |||||
44 | hydrocortisone | 5.57 | 88.0 | 2.11 | 94.1 | 6.97 | 70.4 | 4.53 | |||||
45 | prednisolone | - | 70.3 | 11.9 | 71.7 | 7.36 | 66.2 | 8.19 | |||||
46 | cortisone | - | 98.6 | 7.98 | 90.7 | 4.83 | 84.0 | 3.15 | |||||
47 | prednisone | - | 75.4 | 7.86 | 79.9 | 7.70 | 67.4 | 7.49 | |||||
48 | fluocinolone acetonide | - | 73.0 | 10.2 | 78.7 | 8.51 | 66.0 | 9.31 | |||||
49 | fludrocortisone | - | 77.0 | 3.66 | 78.2 | 6.70 | 66.5 | 7.52 | |||||
50 | beclomethasone | - | 66.1 | 5.21 | 66.7 | 6.19 | 69.1 | 6.11 |
Table 6 Spiked recoveries and precisions of the target compounds in a beef sample (n=6)
No. | Compound | Matrix content/ (μg/kg) | Added levels* | ||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Low | Middle | High | |||||||||||
Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | ||||||||
1 | tulobuterol | - | 102.3 | 2.26 | 105.3 | 3.09 | 89.9 | 5.33 | |||||
2 | clenbuterol | - | 113.7 | 2.83 | 111.5 | 7.83 | 113.9 | 5.31 | |||||
3 | bambuterol | - | 106.0 | 2.50 | 104.7 | 3.79 | 89.3 | 4.77 | |||||
4 | salmeterol | - | 87.7 | 2.37 | 98.6 | 3.03 | 97.3 | 13.2 | |||||
5 | clenproperol | - | 85.7 | 1.35 | 85.1 | 1.49 | 86.8 | 4.38 | |||||
6 | zilpaterol | - | 101.3 | 1.51 | 97.9 | 1.59 | 89.6 | 0.76 | |||||
7 | fenoterol | - | 72.0 | 2.78 | 80.9 | 4.59 | 73.9 | 5.34 | |||||
8 | penbuterol | - | 104.0 | 3.47 | 113.5 | 2.91 | 109.5 | 8.45 | |||||
9 | clencyclohexerol | - | 65.0 | 2.66 | 66.6 | 8.46 | 66.6 | 4.78 | |||||
10 | mabuterol | - | 107.7 | 3.75 | 117.7 | 1.44 | 110.3 | 0.82 | |||||
11 | brombuterol | - | 103.0 | 0.97 | 104.8 | 2.98 | 107.1 | 2.68 | |||||
12 | cimaterol | - | 112.3 | 4.39 | 103.9 | 0.99 | 105.6 | 2.18 | |||||
13 | salbutamol | - | 94.3 | 11.7 | 106.1 | 8.12 | 109.0 | 2.70 | |||||
14 | metaproterenol | - | 67.0 | 8.31 | 84.2 | 4.91 | 84.2 | 2.38 | |||||
15 | terbutaline | - | 95.0 | 5.26 | 102.3 | 8.64 | 97.5 | 10.3 | |||||
16 | clorprenaline | - | 85.0 | 4.71 | 87.9 | 1.25 | 85.0 | 1.19 | |||||
17 | ractopamine | - | 101.0 | 0.99 | 86.2 | 4.96 | 87.1 | 2.52 | |||||
18 | demethyl coclaurine | - | 93.7 | 2.47 | 88.9 | 3.64 | 89.7 | 2.77 | |||||
19 | tretoquinol | - | 84.3 | 3.81 | 84.1 | 1.80 | 87.0 | 1.59 | |||||
20 | atenolol | - | 101.0 | 3.43 | 110.2 | 6.72 | 104.5 | 3.78 | |||||
21 | propranolol | - | 92.6 | 4.52 | 99.8 | 7.01 | 100.6 | 5.01 | |||||
22 | metoprolol | - | 96.6 | 8.75 | 110.5 | 4.22 | 112.9 | 4.47 | |||||
23 | trenbolone | - | 92.3 | 5.20 | 102.7 | 2.97 | 91.9 | 1.78 | |||||
24 | methyltestosterone | - | 107.5 | 6.51 | 111.8 | 4.19 | 74.8 | 2.79 | |||||
25 | boldenone | - | 105.3 | 5.16 | 116.5 | 4.41 | 96.0 | 2.10 | |||||
26 | nortestosterone | - | 86.9 | 8.31 | 90.9 | 4.19 | 78.8 | 2.64 | |||||
27 | stanozolol | - | 51.7 | 5.58 | 54.4 | 2.57 | 52.5 | 3.25 | |||||
28 | methandienone | - | 84.3 | 4.87 | 99.1 | 3.07 | 69.0 | 3.72 | |||||
29 | mesterolone | - | 57.3 | 4.01 | 50.4 | 5.34 | 53.9 | 3.18 | |||||
30 | mestanolone | - | 53.1 | 5.50 | 52.4 | 5.86 | 53.9 | 3.36 | |||||
31 | testosterone | - | 70.1 | 5.44 | 65.8 | 7.24 | 66.0 | 1.60 | |||||
32 | 4-androstene-3 | - | 92.3 | 8.40 | 80.6 | 7.89 | 79.1 | 0.77 | |||||
33 | prasterone | - | 92.2 | 5.92 | 101.2 | 7.18 | 107.5 | 2.18 | |||||
34 | progesterone | 12.0 | 104.6 | 1.99 | 96.6 | 1.47 | 93.0 | 3.22 | |||||
35 | chlormadinone acetate | - | 63.7 | 7.66 | 75.3 | 5.81 | 68.3 | 9.47 | |||||
36 | melengestrol acetate | - | 85.3 | 12.8 | 83.4 | 12.6 | 83.7 | 8.31 | |||||
37 | medroxyprogesterone acetate | - | 90.0 | 7.95 | 93.9 | 3.31 | 97.4 | 3.41 | |||||
38 | 17-α-hydroxyprogesterone | - | 73.4 | 8.58 | 76.1 | 10.1 | 72.2 | 5.32 | |||||
39 | megestrol | - | 60.7 | 8.30 | 71.0 | 4.09 | 74.7 | 3.09 | |||||
40 | triamterene | - | 63.7 | 6.27 | 61.1 | 1.36 | 68.0 | 2.15 | |||||
41 | spironolactone | - | 91.4 | 7.03 | 83.7 | 1.97 | 86.2 | 5.03 | |||||
42 | canrenone | - | 67.3 | 5.22 | 69.1 | 3.95 | 66.5 | 2.90 | |||||
43 | dexamethasone | - | 81.2 | 7.10 | 107.8 | 3.03 | 101.2 | 10.1 | |||||
44 | hydrocortisone | 5.57 | 88.0 | 2.11 | 94.1 | 6.97 | 70.4 | 4.53 | |||||
45 | prednisolone | - | 70.3 | 11.9 | 71.7 | 7.36 | 66.2 | 8.19 | |||||
46 | cortisone | - | 98.6 | 7.98 | 90.7 | 4.83 | 84.0 | 3.15 | |||||
47 | prednisone | - | 75.4 | 7.86 | 79.9 | 7.70 | 67.4 | 7.49 | |||||
48 | fluocinolone acetonide | - | 73.0 | 10.2 | 78.7 | 8.51 | 66.0 | 9.31 | |||||
49 | fludrocortisone | - | 77.0 | 3.66 | 78.2 | 6.70 | 66.5 | 7.52 | |||||
50 | beclomethasone | - | 66.1 | 5.21 | 66.7 | 6.19 | 69.1 | 6.11 |
Sample | This method/(μg/kg) | GB/T 21981-2008/(μg/kg) | ||||||
---|---|---|---|---|---|---|---|---|
Hydrocortisone | Cortisone | 4-Androstene-3 | Hydrocortisone | Cortisone | 4-Androstene-3 | |||
Pork 1 | 4.9 | 1.7 | - | 5.2 | 1.7 | - | ||
Pork 2 | 16.4 | 7.7 | - | 18.4 | 8.1 | - | ||
Pork 3 | 5.6 | 0.9 | - | 6.7 | 1.4 | - | ||
Chicken breast | - | - | - | - | - | - | ||
Chicken wings | - | - | - | - | - | - | ||
Duck | - | - | - | - | - | - | ||
Beef 1 | 5.9 | 0.4 | - | 6.3 | 0.4 | - | ||
Beef 2 | 3.8 | 1.3 | 0.3 | 3.4 | 1.1 | - | ||
Beef 3 | 5.8 | 2.4 | - | 5.7 | 2.0 | - | ||
LOQ/(μg/kg) | 0.4 | 0.4 | 0.2 | 0.4 | 0.4 | 0.4 |
Table 7 Detection results for meat samples by two methods (n=2)
Sample | This method/(μg/kg) | GB/T 21981-2008/(μg/kg) | ||||||
---|---|---|---|---|---|---|---|---|
Hydrocortisone | Cortisone | 4-Androstene-3 | Hydrocortisone | Cortisone | 4-Androstene-3 | |||
Pork 1 | 4.9 | 1.7 | - | 5.2 | 1.7 | - | ||
Pork 2 | 16.4 | 7.7 | - | 18.4 | 8.1 | - | ||
Pork 3 | 5.6 | 0.9 | - | 6.7 | 1.4 | - | ||
Chicken breast | - | - | - | - | - | - | ||
Chicken wings | - | - | - | - | - | - | ||
Duck | - | - | - | - | - | - | ||
Beef 1 | 5.9 | 0.4 | - | 6.3 | 0.4 | - | ||
Beef 2 | 3.8 | 1.3 | 0.3 | 3.4 | 1.1 | - | ||
Beef 3 | 5.8 | 2.4 | - | 5.7 | 2.0 | - | ||
LOQ/(μg/kg) | 0.4 | 0.4 | 0.2 | 0.4 | 0.4 | 0.4 |
Compound | Content range/(μg/kg) | Detection rate/% |
---|---|---|
Hydrocortisone | 3.3-22.6 | 100 |
Cortisone | 1.5-2.1 | 67 |
4-Androstene-3 | 0.7-1.2 | 17 |
Testosterone | 0.6-1.5 | 42 |
Table 8 Detection results for 12 beef samples (n=2)
Compound | Content range/(μg/kg) | Detection rate/% |
---|---|---|
Hydrocortisone | 3.3-22.6 | 100 |
Cortisone | 1.5-2.1 | 67 |
4-Androstene-3 | 0.7-1.2 | 17 |
Testosterone | 0.6-1.5 | 42 |
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