Chinese Journal of Chromatography ›› 2023, Vol. 41 ›› Issue (7): 622-631.DOI: 10.3724/SP.J.1123.2022.11022
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XIE Yingshuang1, WANG Bo1,*(), LEI Chunni1, LIU Lanxia2, ZHANG Huan1, BAI Xingbin1, KOU Zonghong2
Received:
2022-11-26
Online:
2023-07-08
Published:
2023-06-30
Supported by:
CLC Number:
XIE Yingshuang, WANG Bo, LEI Chunni, LIU Lanxia, ZHANG Huan, BAI Xingbin, KOU Zonghong. Determination of 41 veterinary drug residues in livestock and poultry meat using a composite purification system coupled with direct analysis in real time-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2023, 41(7): 622-631.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2022.11022
No. | Compound | Parent ion (m/z) | Daughter ions (m/z) | DP/ V | CEs/ eV | Ion source |
---|---|---|---|---|---|---|
1 | sulfamethazine (磺胺二甲嘧啶) | 279.1 | 186.0*,124.0 | 110 | 15,20 | DART+ |
2 | sulfamethoxazole (磺胺甲基异恶唑) | 254.1 | 108.1*,92.1 | 110 | 35,35 | DART+ |
3 | sulfamonomethoxine (磺胺-6-甲氧嘧啶) | 281.0 | 156.0*,92.0 | 110 | 22,35 | DART+ |
4 | sulfaquinoxaline (磺胺喹恶啉) | 301.1 | 156.0*,92.0 | 130 | 16,30 | DART+ |
5 | sulfadimethoxine (磺胺二甲氧嘧啶) | 311.0 | 156.0*,92.0 | 130 | 20,32 | DART+ |
6 | trimethoprim (甲氧苄啶) | 291.3 | 123.0*,230.2 | 125 | 30,30 | DART+ |
7 | sulfapyridine (磺胺吡啶) | 250.0 | 92.1*,156.1 | 100 | 32,15 | DART+ |
8 | sulfadiazine (磺胺嘧啶) | 251.0 | 156.0*,92.0 | 115 | 15,27 | DART+ |
9 | sulfamethoxazole (磺胺甲恶唑) | 254.1 | 92.1*,108.1 | 110 | 30,30 | DART+ |
10 | sulfathiazole (磺胺噻唑) | 256.0 | 156.1*,92.1 | 100 | 30,15 | DART+ |
11 | sulfamerazine (磺胺甲基嘧啶) | 265.1 | 156.1*,65.1 | 100 | 10,40 | DART+ |
12 | sulfamoxol (磺胺二甲恶唑) | 285.1 | 156.2*,108.0 | 100 | 23,33 | DART+ |
13 | sulfisoxazole (磺胺异恶唑) | 268.1 | 156.0*,113.0 | 115 | 30,13 | DART+ |
14 | sulfamethoxypyridazine (磺胺甲氧哒嗪) | 285.1 | 108.0*,156.0 | 120 | 22,10 | DART+ |
15 | sulfamonomethoxine (磺胺间甲氧嘧啶) | 281.0 | 156.1*,65.1 | 100 | 20,30 | DART+ |
16 | norfloxacin (诺氟沙星) | 320.2 | 302.2*,276.2 | 115 | 15,13 | DART+ |
17 | ofloxacin (氧氟沙星) | 362.2 | 318.2*,261.1 | 135 | 10,30 | DART+ |
18 | pefloxacin (培氟沙星) | 334.2 | 316.2*,70.1 | 115 | 15,45 | DART+ |
19 | ciprofloxacin (环丙沙星) | 332.3 | 288.2*,245.2 | 125 | 15,25 | DART+ |
20 | enrofloxacin (恩诺沙星) | 360.2 | 342.1*,316.1 | 135 | 10,10 | DART+ |
21 | danofloxacin (达氟沙星) | 358.0 | 314.1*,340.1 | 135 | 20,25 | DART+ |
22 | sarafloxacin (沙拉沙星) | 386.3 | 342.2*,299.2 | 140 | 20,30 | DART+ |
23 | difloxacin (二氟沙星) | 400.3 | 356.3*,299.2 | 135 | 20,20 | DART+ |
24 | enoxacin (依诺沙星) | 321.3 | 303.1*,232.1 | 120 | 10,30 | DART+ |
25 | pimonidazole (哌莫硝唑) | 255.0 | 124.3*,98.3 | 110 | 20,15 | DART+ |
26 | hydroxymetronidazole (羟基甲硝唑) | 187.7 | 126.1*,123.1 | 80 | 25,30 | DART+ |
27 | 1-methyl-5-nitro-1H-imidazole-2-methanol (羟基二甲硝咪唑) | 157.9 | 94.3*,55.4 | 80 | 25,25 | DART+ |
28 | metronidazole (甲硝唑) | 172.3 | 127.9*,82.1 | 80 | 10,25 | DART+ |
29 | tinidazole (替硝唑) | 247.8 | 128.2*,82.3 | 90 | 25,20 | DART+ |
30 | 2-dimethyl-5-nitro-1H-imidazole-1-ethanol (塞克硝唑) | 186.1 | 128.2*,82.3 | 90 | 20,25 | DART+ |
31 | 2-methyl-5-nitro-1H-imidazole-1-propanolmonohydrochloride (特尼达唑) | 186.2 | 128.2*,82.3 | 90 | 20,25 | DART+ |
32 | hydroxy-ipronidazole (羟基异丙硝唑) | 185.9 | 168.2*,122.3 | 90 | 20,20 | DART+ |
33 | ipronidazole (异丙硝唑) | 169.8 | 124.1*,109.1 | 85 | 20,20 | DART+ |
34 | benznidazole (苄硝唑) | 261.0 | 107.3*,91.3 | 110 | 15,25 | DART+ |
35 | fexinidazole (非昔硝唑) | 233.1 | 93.3*,106.3 | 110 | 15,25 | DART+ |
36 | panidazole (帕硝唑) | 233.0 | 106.3*,93.3 | 110 | 25,10 | DART+ |
37 | carnidazole (卡硝唑) | 245.0 | 118.2*,75.2 | 110 | 20,10 | DART+ |
38 | misonidazole (米索硝唑) | 202.1 | 145.3*,174.2 | 110 | 25,15 | DART+ |
39 | chloramphenicol (氯霉素) | 321.0 | 152.0*,257.1 | 110 | 11,4 | DART- |
40 | florfenicol (氟苯尼考) | 247.9 | 229.8*,130.1 | 110 | 10,22 | DART- |
41 | thiamphenicol (甲砜霉素) | 354.1 | 185.1*,290.1 | 110 | 17,5 | DART- |
42 | norfloxacin-D5 (诺氟沙星-D5) | 325.0 | 306.9*,280.9 | 100 | 15,15 | DART+ |
43 | ciprofloxacin-D8 (环丙沙星-D8) | 340.1 | 322.1*,234.8 | 80 | 20,40 | DART+ |
44 | enrofloxacin-D5 (恩诺沙星-D5) | 365.3 | 347.2*,321.3 | 125 | 19,15 | DART+ |
45 | sulfadoxine-D3 (磺胺邻二甲氧嘧啶-D3) | 314.0 | 156* | 125 | 17 | DART+ |
46 | sulfadimethoxine-D6 (磺胺间二甲氧基嘧啶-D6) | 317.0 | 156* | 125 | 20 | DART+ |
47 | metronidazole-D3 (甲硝唑-D3) | 175.1 | 127.9* | 80 | 10 | DART+ |
48 | chloramphenicol-D5 (氯霉素-D5) | 325.8 | 156.6* | 130 | 15 | DART- |
49 | tinidazole-D5 (替硝唑-D5) | 253.1 | 126.1* | 110 | 15 | DART+ |
Table 1 Mass spectrometry parameters of the 41 veterinary drugs and eight internal standards
No. | Compound | Parent ion (m/z) | Daughter ions (m/z) | DP/ V | CEs/ eV | Ion source |
---|---|---|---|---|---|---|
1 | sulfamethazine (磺胺二甲嘧啶) | 279.1 | 186.0*,124.0 | 110 | 15,20 | DART+ |
2 | sulfamethoxazole (磺胺甲基异恶唑) | 254.1 | 108.1*,92.1 | 110 | 35,35 | DART+ |
3 | sulfamonomethoxine (磺胺-6-甲氧嘧啶) | 281.0 | 156.0*,92.0 | 110 | 22,35 | DART+ |
4 | sulfaquinoxaline (磺胺喹恶啉) | 301.1 | 156.0*,92.0 | 130 | 16,30 | DART+ |
5 | sulfadimethoxine (磺胺二甲氧嘧啶) | 311.0 | 156.0*,92.0 | 130 | 20,32 | DART+ |
6 | trimethoprim (甲氧苄啶) | 291.3 | 123.0*,230.2 | 125 | 30,30 | DART+ |
7 | sulfapyridine (磺胺吡啶) | 250.0 | 92.1*,156.1 | 100 | 32,15 | DART+ |
8 | sulfadiazine (磺胺嘧啶) | 251.0 | 156.0*,92.0 | 115 | 15,27 | DART+ |
9 | sulfamethoxazole (磺胺甲恶唑) | 254.1 | 92.1*,108.1 | 110 | 30,30 | DART+ |
10 | sulfathiazole (磺胺噻唑) | 256.0 | 156.1*,92.1 | 100 | 30,15 | DART+ |
11 | sulfamerazine (磺胺甲基嘧啶) | 265.1 | 156.1*,65.1 | 100 | 10,40 | DART+ |
12 | sulfamoxol (磺胺二甲恶唑) | 285.1 | 156.2*,108.0 | 100 | 23,33 | DART+ |
13 | sulfisoxazole (磺胺异恶唑) | 268.1 | 156.0*,113.0 | 115 | 30,13 | DART+ |
14 | sulfamethoxypyridazine (磺胺甲氧哒嗪) | 285.1 | 108.0*,156.0 | 120 | 22,10 | DART+ |
15 | sulfamonomethoxine (磺胺间甲氧嘧啶) | 281.0 | 156.1*,65.1 | 100 | 20,30 | DART+ |
16 | norfloxacin (诺氟沙星) | 320.2 | 302.2*,276.2 | 115 | 15,13 | DART+ |
17 | ofloxacin (氧氟沙星) | 362.2 | 318.2*,261.1 | 135 | 10,30 | DART+ |
18 | pefloxacin (培氟沙星) | 334.2 | 316.2*,70.1 | 115 | 15,45 | DART+ |
19 | ciprofloxacin (环丙沙星) | 332.3 | 288.2*,245.2 | 125 | 15,25 | DART+ |
20 | enrofloxacin (恩诺沙星) | 360.2 | 342.1*,316.1 | 135 | 10,10 | DART+ |
21 | danofloxacin (达氟沙星) | 358.0 | 314.1*,340.1 | 135 | 20,25 | DART+ |
22 | sarafloxacin (沙拉沙星) | 386.3 | 342.2*,299.2 | 140 | 20,30 | DART+ |
23 | difloxacin (二氟沙星) | 400.3 | 356.3*,299.2 | 135 | 20,20 | DART+ |
24 | enoxacin (依诺沙星) | 321.3 | 303.1*,232.1 | 120 | 10,30 | DART+ |
25 | pimonidazole (哌莫硝唑) | 255.0 | 124.3*,98.3 | 110 | 20,15 | DART+ |
26 | hydroxymetronidazole (羟基甲硝唑) | 187.7 | 126.1*,123.1 | 80 | 25,30 | DART+ |
27 | 1-methyl-5-nitro-1H-imidazole-2-methanol (羟基二甲硝咪唑) | 157.9 | 94.3*,55.4 | 80 | 25,25 | DART+ |
28 | metronidazole (甲硝唑) | 172.3 | 127.9*,82.1 | 80 | 10,25 | DART+ |
29 | tinidazole (替硝唑) | 247.8 | 128.2*,82.3 | 90 | 25,20 | DART+ |
30 | 2-dimethyl-5-nitro-1H-imidazole-1-ethanol (塞克硝唑) | 186.1 | 128.2*,82.3 | 90 | 20,25 | DART+ |
31 | 2-methyl-5-nitro-1H-imidazole-1-propanolmonohydrochloride (特尼达唑) | 186.2 | 128.2*,82.3 | 90 | 20,25 | DART+ |
32 | hydroxy-ipronidazole (羟基异丙硝唑) | 185.9 | 168.2*,122.3 | 90 | 20,20 | DART+ |
33 | ipronidazole (异丙硝唑) | 169.8 | 124.1*,109.1 | 85 | 20,20 | DART+ |
34 | benznidazole (苄硝唑) | 261.0 | 107.3*,91.3 | 110 | 15,25 | DART+ |
35 | fexinidazole (非昔硝唑) | 233.1 | 93.3*,106.3 | 110 | 15,25 | DART+ |
36 | panidazole (帕硝唑) | 233.0 | 106.3*,93.3 | 110 | 25,10 | DART+ |
37 | carnidazole (卡硝唑) | 245.0 | 118.2*,75.2 | 110 | 20,10 | DART+ |
38 | misonidazole (米索硝唑) | 202.1 | 145.3*,174.2 | 110 | 25,15 | DART+ |
39 | chloramphenicol (氯霉素) | 321.0 | 152.0*,257.1 | 110 | 11,4 | DART- |
40 | florfenicol (氟苯尼考) | 247.9 | 229.8*,130.1 | 110 | 10,22 | DART- |
41 | thiamphenicol (甲砜霉素) | 354.1 | 185.1*,290.1 | 110 | 17,5 | DART- |
42 | norfloxacin-D5 (诺氟沙星-D5) | 325.0 | 306.9*,280.9 | 100 | 15,15 | DART+ |
43 | ciprofloxacin-D8 (环丙沙星-D8) | 340.1 | 322.1*,234.8 | 80 | 20,40 | DART+ |
44 | enrofloxacin-D5 (恩诺沙星-D5) | 365.3 | 347.2*,321.3 | 125 | 19,15 | DART+ |
45 | sulfadoxine-D3 (磺胺邻二甲氧嘧啶-D3) | 314.0 | 156* | 125 | 17 | DART+ |
46 | sulfadimethoxine-D6 (磺胺间二甲氧基嘧啶-D6) | 317.0 | 156* | 125 | 20 | DART+ |
47 | metronidazole-D3 (甲硝唑-D3) | 175.1 | 127.9* | 80 | 10 | DART+ |
48 | chloramphenicol-D5 (氯霉素-D5) | 325.8 | 156.6* | 130 | 15 | DART- |
49 | tinidazole-D5 (替硝唑-D5) | 253.1 | 126.1* | 110 | 15 | DART+ |
K | Maximum allowable deviation range/% |
---|---|
K>50 | ±20 |
20<K≤50 | ±25 |
10<K≤20 | ±30 |
K≤10 | ±50 |
Table 2 Maximum allowable deviation ranges of relative ion abundance (K) in mass spectrometry
K | Maximum allowable deviation range/% |
---|---|
K>50 | ±20 |
20<K≤50 | ±25 |
10<K≤20 | ±30 |
K≤10 | ±50 |
No. | Compound | Linear range/ (μg/L) | r | LOD/ (μg/kg) | LOQ/ (μg/kg) | No. | Compound | Linear range/ (μg/L) | r | LOD/ (μg/kg) | LOQ/ (μg/kg) |
---|---|---|---|---|---|---|---|---|---|---|---|
1 | sulfadimidine | 2-200 | 0.9993 | 0.5 | 2.0 | 24 | enoxacin | 2-200 | 0.9998 | 0.5 | 2.0 |
2 | sulfamethoxazole | 2-200 | 0.9998 | 0.5 | 2.0 | 25 | garms nitrous oxide | 2-200 | 0.9995 | 0.5 | 2.0 |
3 | sulfamonomethoxine | 2-200 | 0.9995 | 0.5 | 2.0 | 26 | hydroxymetronidazole | 2-200 | 0.9998 | 0.5 | 2.0 |
4 | sulfaquinoxaline | 2-200 | 0.9998 | 0.5 | 2.0 | 27 | 1-methyl-5-nitro-1H- | 2-200 | 0.9996 | 0.5 | 2.0 |
5 | sulfadimethoxine | 2-200 | 0.9997 | 0.5 | 2.0 | imidazole-2-methanol | |||||
6 | trimethoprim | 2-200 | 0.9998 | 0.5 | 2.0 | 28 | metronidazole | 2-200 | 0.9998 | 0.5 | 2.0 |
7 | sulfapyridine | 2-200 | 0.9979 | 0.5 | 2.0 | 29 | tinidazole | 2-200 | 0.9996 | 0.5 | 2.0 |
8 | sulfadiazine | 2-200 | 0.9990 | 0.5 | 2.0 | 30 | 2-dimethyl-5-nitro-1H- | 2-200 | 0.9998 | 0.5 | 2.0 |
9 | sulfamethoxazole | 2-200 | 0.9999 | 0.5 | 2.0 | imidazole-1-ethanol | |||||
10 | sulfathiazole | 2-200 | 0.9997 | 0.5 | 2.0 | 31 | 2-methyl-5-nitro-1H- | 2-200 | 0.9996 | 0.5 | 2.0 |
11 | sulfamethyldiazine | 2-200 | 0.9998 | 0.5 | 2.0 | imidazole-1-propanol | |||||
12 | sulfamethazole | 2-200 | 0.9998 | 0.5 | 2.0 | monohydrochloride | |||||
13 | sulfisoxazole | 2-200 | 0.9987 | 0.5 | 2.0 | 32 | hydroxy-ipronidazole | 2-200 | 0.9998 | 0.5 | 2.0 |
14 | sulfamethoxypyridazine | 2-200 | 0.9994 | 0.5 | 2.0 | 33 | ipronidazole | 2-200 | 0.9997 | 0.5 | 2.0 |
15 | sulfamonomethoxine | 2-200 | 0.9997 | 0.5 | 2.0 | 34 | benznidazole | 2-200 | 0.9998 | 0.5 | 2.0 |
16 | norfloxacin | 2-200 | 0.9998 | 0.5 | 2.0 | 35 | fexinidazole | 2-200 | 0.9995 | 0.5 | 2.0 |
17 | ofloxacin | 2-200 | 0.9996 | 0.5 | 2.0 | 36 | panidazole | 2-200 | 0.9998 | 0.5 | 2.0 |
18 | peflacine | 2-200 | 0.9995 | 0.5 | 2.0 | 37 | carnidazole | 2-200 | 0.9996 | 0.5 | 2.0 |
19 | ciprofloxacin | 2-200 | 0.9999 | 0.5 | 2.0 | 38 | misonidazole | 2-200 | 0.9998 | 0.5 | 2.0 |
20 | ennosault | 2-200 | 0.9999 | 0.5 | 2.0 | 39 | chloramphenicol | 0.5-20 | 0.9995 | 0.1 | 0.5 |
21 | danofloxacin | 2-200 | 0.9996 | 0.5 | 2.0 | 40 | florfenicol | 0.5-20 | 0.9997 | 0.1 | 0.5 |
22 | sarafloxacin | 2-200 | 0.9998 | 0.5 | 2.0 | 41 | thiamphenicol | 0.5-20 | 0.9996 | 0.1 | 0.5 |
23 | difloxacin | 2-200 | 0.9996 | 0.5 | 2.0 |
Table 3 Linear ranges, correlation coefficients (r), LODs and LOQs of the 41 veterinary drugs in pork matrix (n=6)
No. | Compound | Linear range/ (μg/L) | r | LOD/ (μg/kg) | LOQ/ (μg/kg) | No. | Compound | Linear range/ (μg/L) | r | LOD/ (μg/kg) | LOQ/ (μg/kg) |
---|---|---|---|---|---|---|---|---|---|---|---|
1 | sulfadimidine | 2-200 | 0.9993 | 0.5 | 2.0 | 24 | enoxacin | 2-200 | 0.9998 | 0.5 | 2.0 |
2 | sulfamethoxazole | 2-200 | 0.9998 | 0.5 | 2.0 | 25 | garms nitrous oxide | 2-200 | 0.9995 | 0.5 | 2.0 |
3 | sulfamonomethoxine | 2-200 | 0.9995 | 0.5 | 2.0 | 26 | hydroxymetronidazole | 2-200 | 0.9998 | 0.5 | 2.0 |
4 | sulfaquinoxaline | 2-200 | 0.9998 | 0.5 | 2.0 | 27 | 1-methyl-5-nitro-1H- | 2-200 | 0.9996 | 0.5 | 2.0 |
5 | sulfadimethoxine | 2-200 | 0.9997 | 0.5 | 2.0 | imidazole-2-methanol | |||||
6 | trimethoprim | 2-200 | 0.9998 | 0.5 | 2.0 | 28 | metronidazole | 2-200 | 0.9998 | 0.5 | 2.0 |
7 | sulfapyridine | 2-200 | 0.9979 | 0.5 | 2.0 | 29 | tinidazole | 2-200 | 0.9996 | 0.5 | 2.0 |
8 | sulfadiazine | 2-200 | 0.9990 | 0.5 | 2.0 | 30 | 2-dimethyl-5-nitro-1H- | 2-200 | 0.9998 | 0.5 | 2.0 |
9 | sulfamethoxazole | 2-200 | 0.9999 | 0.5 | 2.0 | imidazole-1-ethanol | |||||
10 | sulfathiazole | 2-200 | 0.9997 | 0.5 | 2.0 | 31 | 2-methyl-5-nitro-1H- | 2-200 | 0.9996 | 0.5 | 2.0 |
11 | sulfamethyldiazine | 2-200 | 0.9998 | 0.5 | 2.0 | imidazole-1-propanol | |||||
12 | sulfamethazole | 2-200 | 0.9998 | 0.5 | 2.0 | monohydrochloride | |||||
13 | sulfisoxazole | 2-200 | 0.9987 | 0.5 | 2.0 | 32 | hydroxy-ipronidazole | 2-200 | 0.9998 | 0.5 | 2.0 |
14 | sulfamethoxypyridazine | 2-200 | 0.9994 | 0.5 | 2.0 | 33 | ipronidazole | 2-200 | 0.9997 | 0.5 | 2.0 |
15 | sulfamonomethoxine | 2-200 | 0.9997 | 0.5 | 2.0 | 34 | benznidazole | 2-200 | 0.9998 | 0.5 | 2.0 |
16 | norfloxacin | 2-200 | 0.9998 | 0.5 | 2.0 | 35 | fexinidazole | 2-200 | 0.9995 | 0.5 | 2.0 |
17 | ofloxacin | 2-200 | 0.9996 | 0.5 | 2.0 | 36 | panidazole | 2-200 | 0.9998 | 0.5 | 2.0 |
18 | peflacine | 2-200 | 0.9995 | 0.5 | 2.0 | 37 | carnidazole | 2-200 | 0.9996 | 0.5 | 2.0 |
19 | ciprofloxacin | 2-200 | 0.9999 | 0.5 | 2.0 | 38 | misonidazole | 2-200 | 0.9998 | 0.5 | 2.0 |
20 | ennosault | 2-200 | 0.9999 | 0.5 | 2.0 | 39 | chloramphenicol | 0.5-20 | 0.9995 | 0.1 | 0.5 |
21 | danofloxacin | 2-200 | 0.9996 | 0.5 | 2.0 | 40 | florfenicol | 0.5-20 | 0.9997 | 0.1 | 0.5 |
22 | sarafloxacin | 2-200 | 0.9998 | 0.5 | 2.0 | 41 | thiamphenicol | 0.5-20 | 0.9996 | 0.1 | 0.5 |
23 | difloxacin | 2-200 | 0.9996 | 0.5 | 2.0 |
Compound | 2.0 μg/kg | 10.0 μg/kg | 20.0 μg/kg | |||||||||||||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Recovery/ % | RSD/ % | Intra- day RSD/% | Inter- day RSD/%# | Recovery/ % | RSD/ % | Intra- day RSD/% | Inter- day RSD/%# | Recovery/ % | RSD/ % | Intra- day RSD/% | Inter- day RSD/%# | |||||||||||||||||
Sulfadimidine | 82.4 | 5.7 | 4.3 | 2.3 | 87.5 | 2.4 | 2.1 | 3.3 | 82.6 | 3.2 | 3.6 | 3.5 | ||||||||||||||||
Sulfamethoxazole | 93.2 | 5.9 | 2.8 | 2.9 | 90.2 | 1.5 | 3.2 | 3.5 | 98.2 | 4.1 | 2.9 | 3.4 | ||||||||||||||||
Sulfamonomethoxine | 97.0 | 4.8 | 1.5 | 3.1 | 85.8 | 4.5 | 3.1 | 3.8 | 82.6 | 4.1 | 3.5 | 2.8 | ||||||||||||||||
Sulfaquinoxaline | 93.2 | 4.5 | 4.1 | 2.9 | 84.2 | 3.6 | 2.6 | 3.2 | 85.6 | 3.2 | 2.9 | 4.2 | ||||||||||||||||
Sulfadimethoxine | 95.6 | 3.7 | 3.2 | 4.2 | 88.5 | 4.5 | 2.6 | 3.2 | 95.2 | 2.1 | 2.4 | 3.1 | ||||||||||||||||
Trimethoprim | 86.5 | 4.0 | 3.2 | 6.3 | 98.6 | 2.8 | 3.2 | 4.1 | 93.6 | 3.5 | 3.5 | 3.9 | ||||||||||||||||
Sulfapyridine | 88.0 | 3.8 | 4.2 | 3.6 | 81.1 | 4.8 | 2.8 | 5.4 | 89.9 | 2.5 | 4.6 | 3.0 | ||||||||||||||||
Sulfadiazine | 89.4 | 3.2 | 3.5 | 3.9 | 88.9 | 2.7 | 3.8 | 3.9 | 96.3 | 3.6 | 6.2 | 2.9 | ||||||||||||||||
Sulfamethoxazole | 92.6 | 3.3 | 3.1 | 3.6 | 91.9 | 4.3 | 1.8 | 4.3 | 97.2 | 3.8 | 4.1 | 6.8 | ||||||||||||||||
Sulfathiazole | 83.7 | 4.2 | 3.9 | 2.3 | 80.6 | 2.4 | 1.7 | 4.4 | 87.9 | 1.3 | 2.4 | 6.6 | ||||||||||||||||
Sulfamethyldiazine | 85.8 | 6.9 | 1.9 | 1.3 | 90.2 | 5.6 | 1.1 | 3.2 | 87.1 | 3.1 | 2.4 | 2.5 | ||||||||||||||||
Sulfamethazole | 90.8 | 6.3 | 2.3 | 4.9 | 85.4 | 3.8 | 0.9 | 5.2 | 106.0 | 3.6 | 2.2 | 5.1 | ||||||||||||||||
Sulfisoxazole | 100.2 | 3.5 | 1.1 | 2.3 | 92.6 | 4.6 | 1.6 | 3.8 | 95.6 | 4.4 | 4.1 | 3.3 | ||||||||||||||||
Sulfamethoxypyridazine | 87.9 | 5.2 | 0.9 | 3.2 | 96.2 | 3.2 | 3.4 | 6.6 | 95.6 | 3.6 | 2.6 | 2.1 | ||||||||||||||||
Sulfamonomethoxine | 94.5 | 2.8 | 1.1 | 4.8 | 84.7 | 1.2 | 2.9 | 4.2 | 99.2 | 2.8 | 4.6 | 3.3 | ||||||||||||||||
Norfloxacin | 96.3 | 6.5 | 2.6 | 2.5 | 88.8 | 2.9 | 4.6 | 5.3 | 85.4 | 3.6 | 3.3 | 3.3 | ||||||||||||||||
Ofloxacin | 89.8 | 3.9 | 4.9 | 3.2 | 97.1 | 2.2 | 2.6 | 3.5 | 99.5 | 3.9 | 3.2 | 4.1 | ||||||||||||||||
Peflacine | 84.9 | 4.2 | 5.6 | 2.7 | 85.9 | 2.4 | 6.3 | 2.2 | 102.0 | 4.2 | 2.6 | 3.7 | ||||||||||||||||
Ciprofloxacin | 90.0 | 1.2 | 3.1 | 1.9 | 90.6 | 1.5 | 3.9 | 2.2 | 85.6 | 2.6 | 3.6 | 2.9 | ||||||||||||||||
Ennosault | 97.4 | 3.9 | 6.2 | 3.6 | 88.1 | 4.5 | 5.2 | 3.2 | 98.2 | 2.9 | 2.9 | 2.6 | ||||||||||||||||
Danofloxacin | 96.8 | 2.8 | 4.2 | 4.1 | 96.7 | 5.6 | 3.3 | 2.5 | 101.0 | 3.2 | 3.5 | 4.6 | ||||||||||||||||
Sarafloxacin | 101.0 | 2.1 | 4.3 | 5.9 | 85.1 | 4.7 | 0.9 | 3.7 | 89.5 | 3.5 | 2.9 | 3.2 | ||||||||||||||||
Difloxacin | 97.9 | 3.2 | 1.2 | 4.1 | 103.6 | 1.8 | 1.6 | 3.1 | 85.6 | 4.5 | 2.4 | 5.2 | ||||||||||||||||
Enoxacin | 96.5 | 3.5 | 3.1 | 3.6 | 108.0 | 5.6 | 3.4 | 1.8 | 91.7 | 4.5 | 3.5 | 3.5 | ||||||||||||||||
Garms nitrous oxide | 81.5 | 4.7 | 1.9 | 5.2 | 86.2 | 3.7 | 2.9 | 2.9 | 92.6 | 4.3 | 4.6 | 3.7 | ||||||||||||||||
Hydroxymetronidazole | 109.1 | 4.6 | 2.0 | 6.0 | 92.5 | 3.4 | 4.6 | 3.8 | 88.1 | 1.3 | 6.2 | 3.2 | ||||||||||||||||
1-Methyl-5-nitro-1H- | 100.9 | 4.3 | 2.3 | 3.3 | 97.7 | 4.7 | 2.6 | 2.5 | 100.1 | 1.9 | 4.1 | 3.3 | ||||||||||||||||
imidazole-2-methanol | ||||||||||||||||||||||||||||
Metronidazole | 83.5 | 3.9 | 1.8 | 6.5 | 86.2 | 3.6 | 6.3 | 2.8 | 89.8 | 1.6 | 2.1 | 2.0 | ||||||||||||||||
Tinidazole | 97.6 | 3.8 | 1.5 | 4.6 | 92.5 | 3.8 | 3.9 | 4.2 | 91.8 | 4.9 | 2.9 | 4.2 | ||||||||||||||||
2-Dimethyl-5-nitro-1H- | 95.7 | 3.2 | 2.8 | 5.9 | 97.7 | 4.6 | 5.2 | 2.4 | 87.4 | 2.3 | 1.1 | 3.6 | ||||||||||||||||
imidazole-1-ethanol | ||||||||||||||||||||||||||||
2-Methyl-5-nitro-1H- | 89.5 | 3.3 | 1.7 | 3.3 | 86.5 | 4.3 | 3.3 | 3.1 | 86.3 | 2.6 | 5.4 | 4.1 | ||||||||||||||||
imidazole-1-propanol | ||||||||||||||||||||||||||||
monohydrochloride | ||||||||||||||||||||||||||||
Hydroxy-ipronidazole | 100.1 | 4.2 | 0.9 | 3.2 | 90.2 | 3.8 | 2.1 | 2.6 | 90.6 | 1.5 | 2.4 | 2.6 | ||||||||||||||||
Ipronidazole | 91.2 | 6.9 | 1.2 | 5.0 | 92.3 | 3.6 | 3.2 | 2.9 | 100.6 | 1.3 | 2.2 | 3.3 | ||||||||||||||||
Benznidazole | 95.3 | 6.3 | 1.4 | 4.6 | 92.6 | 3.5 | 3.1 | 2.6 | 93.3 | 2.6 | 4.1 | 3.6 | ||||||||||||||||
Fexinidazole | 94.2 | 3.5 | 1.1 | 3.8 | 92.5 | 4.9 | 2.6 | 3.3 | 88.4 | 3.2 | 2.6 | 2.7 | ||||||||||||||||
Panidazole | 82.2 | 4.8 | 0.9 | 5.6 | 96.5 | 3.7 | 2.6 | 4.3 | 94.9 | 2.8 | 4.6 | 3.9 | ||||||||||||||||
Carnidazole | 93.4 | 5.7 | 2.1 | 3.6 | 86.5 | 3.4 | 3.2 | 2.8 | 95.4 | 3.6 | 3.3 | 4.3 | ||||||||||||||||
Misonidazole | 97.8 | 2.7 | 3.6 | 2.9 | 100.1 | 2.2 | 2.8 | 3.6 | 85.5 | 3.4 | 3.2 | 4.2 | ||||||||||||||||
Chloramphenicol* | 93.5 | 4.5 | 1.6 | 1.3 | 80.7 | 2.7 | 3.8 | 3.1 | 97.2 | 2.6 | 2.6 | 3.9 | ||||||||||||||||
Florfenicol* | 99.5 | 4.9 | 1.9 | 2.1 | 85.2 | 4.0 | 1.8 | 2.5 | 87.9 | 1.4 | 4.1 | 4.3 | ||||||||||||||||
Thiamphenicol* | 99.8 | 3.1 | 6.3 | 2.3 | 96.3 | 4.3 | 1.5 | 0.9 | 95.6 | 3.4 | 2.4 | 3.6 |
Table 4 Recoveries and precisions of the 41 veterinary drugs in pork samples at different spiked levels (n=6)
Compound | 2.0 μg/kg | 10.0 μg/kg | 20.0 μg/kg | |||||||||||||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Recovery/ % | RSD/ % | Intra- day RSD/% | Inter- day RSD/%# | Recovery/ % | RSD/ % | Intra- day RSD/% | Inter- day RSD/%# | Recovery/ % | RSD/ % | Intra- day RSD/% | Inter- day RSD/%# | |||||||||||||||||
Sulfadimidine | 82.4 | 5.7 | 4.3 | 2.3 | 87.5 | 2.4 | 2.1 | 3.3 | 82.6 | 3.2 | 3.6 | 3.5 | ||||||||||||||||
Sulfamethoxazole | 93.2 | 5.9 | 2.8 | 2.9 | 90.2 | 1.5 | 3.2 | 3.5 | 98.2 | 4.1 | 2.9 | 3.4 | ||||||||||||||||
Sulfamonomethoxine | 97.0 | 4.8 | 1.5 | 3.1 | 85.8 | 4.5 | 3.1 | 3.8 | 82.6 | 4.1 | 3.5 | 2.8 | ||||||||||||||||
Sulfaquinoxaline | 93.2 | 4.5 | 4.1 | 2.9 | 84.2 | 3.6 | 2.6 | 3.2 | 85.6 | 3.2 | 2.9 | 4.2 | ||||||||||||||||
Sulfadimethoxine | 95.6 | 3.7 | 3.2 | 4.2 | 88.5 | 4.5 | 2.6 | 3.2 | 95.2 | 2.1 | 2.4 | 3.1 | ||||||||||||||||
Trimethoprim | 86.5 | 4.0 | 3.2 | 6.3 | 98.6 | 2.8 | 3.2 | 4.1 | 93.6 | 3.5 | 3.5 | 3.9 | ||||||||||||||||
Sulfapyridine | 88.0 | 3.8 | 4.2 | 3.6 | 81.1 | 4.8 | 2.8 | 5.4 | 89.9 | 2.5 | 4.6 | 3.0 | ||||||||||||||||
Sulfadiazine | 89.4 | 3.2 | 3.5 | 3.9 | 88.9 | 2.7 | 3.8 | 3.9 | 96.3 | 3.6 | 6.2 | 2.9 | ||||||||||||||||
Sulfamethoxazole | 92.6 | 3.3 | 3.1 | 3.6 | 91.9 | 4.3 | 1.8 | 4.3 | 97.2 | 3.8 | 4.1 | 6.8 | ||||||||||||||||
Sulfathiazole | 83.7 | 4.2 | 3.9 | 2.3 | 80.6 | 2.4 | 1.7 | 4.4 | 87.9 | 1.3 | 2.4 | 6.6 | ||||||||||||||||
Sulfamethyldiazine | 85.8 | 6.9 | 1.9 | 1.3 | 90.2 | 5.6 | 1.1 | 3.2 | 87.1 | 3.1 | 2.4 | 2.5 | ||||||||||||||||
Sulfamethazole | 90.8 | 6.3 | 2.3 | 4.9 | 85.4 | 3.8 | 0.9 | 5.2 | 106.0 | 3.6 | 2.2 | 5.1 | ||||||||||||||||
Sulfisoxazole | 100.2 | 3.5 | 1.1 | 2.3 | 92.6 | 4.6 | 1.6 | 3.8 | 95.6 | 4.4 | 4.1 | 3.3 | ||||||||||||||||
Sulfamethoxypyridazine | 87.9 | 5.2 | 0.9 | 3.2 | 96.2 | 3.2 | 3.4 | 6.6 | 95.6 | 3.6 | 2.6 | 2.1 | ||||||||||||||||
Sulfamonomethoxine | 94.5 | 2.8 | 1.1 | 4.8 | 84.7 | 1.2 | 2.9 | 4.2 | 99.2 | 2.8 | 4.6 | 3.3 | ||||||||||||||||
Norfloxacin | 96.3 | 6.5 | 2.6 | 2.5 | 88.8 | 2.9 | 4.6 | 5.3 | 85.4 | 3.6 | 3.3 | 3.3 | ||||||||||||||||
Ofloxacin | 89.8 | 3.9 | 4.9 | 3.2 | 97.1 | 2.2 | 2.6 | 3.5 | 99.5 | 3.9 | 3.2 | 4.1 | ||||||||||||||||
Peflacine | 84.9 | 4.2 | 5.6 | 2.7 | 85.9 | 2.4 | 6.3 | 2.2 | 102.0 | 4.2 | 2.6 | 3.7 | ||||||||||||||||
Ciprofloxacin | 90.0 | 1.2 | 3.1 | 1.9 | 90.6 | 1.5 | 3.9 | 2.2 | 85.6 | 2.6 | 3.6 | 2.9 | ||||||||||||||||
Ennosault | 97.4 | 3.9 | 6.2 | 3.6 | 88.1 | 4.5 | 5.2 | 3.2 | 98.2 | 2.9 | 2.9 | 2.6 | ||||||||||||||||
Danofloxacin | 96.8 | 2.8 | 4.2 | 4.1 | 96.7 | 5.6 | 3.3 | 2.5 | 101.0 | 3.2 | 3.5 | 4.6 | ||||||||||||||||
Sarafloxacin | 101.0 | 2.1 | 4.3 | 5.9 | 85.1 | 4.7 | 0.9 | 3.7 | 89.5 | 3.5 | 2.9 | 3.2 | ||||||||||||||||
Difloxacin | 97.9 | 3.2 | 1.2 | 4.1 | 103.6 | 1.8 | 1.6 | 3.1 | 85.6 | 4.5 | 2.4 | 5.2 | ||||||||||||||||
Enoxacin | 96.5 | 3.5 | 3.1 | 3.6 | 108.0 | 5.6 | 3.4 | 1.8 | 91.7 | 4.5 | 3.5 | 3.5 | ||||||||||||||||
Garms nitrous oxide | 81.5 | 4.7 | 1.9 | 5.2 | 86.2 | 3.7 | 2.9 | 2.9 | 92.6 | 4.3 | 4.6 | 3.7 | ||||||||||||||||
Hydroxymetronidazole | 109.1 | 4.6 | 2.0 | 6.0 | 92.5 | 3.4 | 4.6 | 3.8 | 88.1 | 1.3 | 6.2 | 3.2 | ||||||||||||||||
1-Methyl-5-nitro-1H- | 100.9 | 4.3 | 2.3 | 3.3 | 97.7 | 4.7 | 2.6 | 2.5 | 100.1 | 1.9 | 4.1 | 3.3 | ||||||||||||||||
imidazole-2-methanol | ||||||||||||||||||||||||||||
Metronidazole | 83.5 | 3.9 | 1.8 | 6.5 | 86.2 | 3.6 | 6.3 | 2.8 | 89.8 | 1.6 | 2.1 | 2.0 | ||||||||||||||||
Tinidazole | 97.6 | 3.8 | 1.5 | 4.6 | 92.5 | 3.8 | 3.9 | 4.2 | 91.8 | 4.9 | 2.9 | 4.2 | ||||||||||||||||
2-Dimethyl-5-nitro-1H- | 95.7 | 3.2 | 2.8 | 5.9 | 97.7 | 4.6 | 5.2 | 2.4 | 87.4 | 2.3 | 1.1 | 3.6 | ||||||||||||||||
imidazole-1-ethanol | ||||||||||||||||||||||||||||
2-Methyl-5-nitro-1H- | 89.5 | 3.3 | 1.7 | 3.3 | 86.5 | 4.3 | 3.3 | 3.1 | 86.3 | 2.6 | 5.4 | 4.1 | ||||||||||||||||
imidazole-1-propanol | ||||||||||||||||||||||||||||
monohydrochloride | ||||||||||||||||||||||||||||
Hydroxy-ipronidazole | 100.1 | 4.2 | 0.9 | 3.2 | 90.2 | 3.8 | 2.1 | 2.6 | 90.6 | 1.5 | 2.4 | 2.6 | ||||||||||||||||
Ipronidazole | 91.2 | 6.9 | 1.2 | 5.0 | 92.3 | 3.6 | 3.2 | 2.9 | 100.6 | 1.3 | 2.2 | 3.3 | ||||||||||||||||
Benznidazole | 95.3 | 6.3 | 1.4 | 4.6 | 92.6 | 3.5 | 3.1 | 2.6 | 93.3 | 2.6 | 4.1 | 3.6 | ||||||||||||||||
Fexinidazole | 94.2 | 3.5 | 1.1 | 3.8 | 92.5 | 4.9 | 2.6 | 3.3 | 88.4 | 3.2 | 2.6 | 2.7 | ||||||||||||||||
Panidazole | 82.2 | 4.8 | 0.9 | 5.6 | 96.5 | 3.7 | 2.6 | 4.3 | 94.9 | 2.8 | 4.6 | 3.9 | ||||||||||||||||
Carnidazole | 93.4 | 5.7 | 2.1 | 3.6 | 86.5 | 3.4 | 3.2 | 2.8 | 95.4 | 3.6 | 3.3 | 4.3 | ||||||||||||||||
Misonidazole | 97.8 | 2.7 | 3.6 | 2.9 | 100.1 | 2.2 | 2.8 | 3.6 | 85.5 | 3.4 | 3.2 | 4.2 | ||||||||||||||||
Chloramphenicol* | 93.5 | 4.5 | 1.6 | 1.3 | 80.7 | 2.7 | 3.8 | 3.1 | 97.2 | 2.6 | 2.6 | 3.9 | ||||||||||||||||
Florfenicol* | 99.5 | 4.9 | 1.9 | 2.1 | 85.2 | 4.0 | 1.8 | 2.5 | 87.9 | 1.4 | 4.1 | 4.3 | ||||||||||||||||
Thiamphenicol* | 99.8 | 3.1 | 6.3 | 2.3 | 96.3 | 4.3 | 1.5 | 0.9 | 95.6 | 3.4 | 2.4 | 3.6 |
Sample number | Sample | Compound | Contents/(μg/kg) | ||
---|---|---|---|---|---|
Original value | This method | National standard method | |||
CSGM-05 | pork | sulfadiazine | / | 89.2 | 90.0 |
CSGM-13 | pork | sulfadiazine | / | 78.1 | 78.0 |
CSGM-18 | pork | sulfadiazine | / | 105.3 | 105.2 |
CSGM-01 | chicken | sarafloxacin | / | 56.3 | 56.4 |
CSGM-07 | chicken | sarafloxacin | / | 102.0 | 102.0 |
LYFC-01 | chicken | metronidazole | 128.2 | 127.8 | 128.1 |
LYFC-01 | pork | ennosault | 312.0 | 311.0 | 320.0 |
LYFC-02 | pork | sarafloxacin | 102.0 | 101.9 | 102.3 |
LYFC-01 | mutton | sulfadiazine | 98.5 | 98.4 | 98.6 |
Table 5 Determination results of actual samples using different detection methods
Sample number | Sample | Compound | Contents/(μg/kg) | ||
---|---|---|---|---|---|
Original value | This method | National standard method | |||
CSGM-05 | pork | sulfadiazine | / | 89.2 | 90.0 |
CSGM-13 | pork | sulfadiazine | / | 78.1 | 78.0 |
CSGM-18 | pork | sulfadiazine | / | 105.3 | 105.2 |
CSGM-01 | chicken | sarafloxacin | / | 56.3 | 56.4 |
CSGM-07 | chicken | sarafloxacin | / | 102.0 | 102.0 |
LYFC-01 | chicken | metronidazole | 128.2 | 127.8 | 128.1 |
LYFC-01 | pork | ennosault | 312.0 | 311.0 | 320.0 |
LYFC-02 | pork | sarafloxacin | 102.0 | 101.9 | 102.3 |
LYFC-01 | mutton | sulfadiazine | 98.5 | 98.4 | 98.6 |
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[1] | DONG Chanchan, HU Yanyun, LÜ Yaning, SONG Wei, HAN Fang, ZHENG Ping, DENG Ning. Magnetic graphene based dispersive micro-solid-phase extraction coupled with liquid chromatography-tandem quadrupole mass spectrometry for the analysis of nine non-steroidal anti-inflammatory drugs in livestock and poultry meat [J]. Chinese Journal of Chromatography, 2016, 34(9): 850-859. |
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