色谱 ›› 2021, Vol. 39 ›› Issue (4): 406-414.DOI: 10.3724/SP.J.1123.2020.05012
收稿日期:
2020-05-29
出版日期:
2021-04-08
发布日期:
2021-03-08
通讯作者:
刘柏林
作者简介:
*E-mail: liubolin087@163.com.
LIU Bolin*(), XIE Jian, ZHAO Ziwei, WANG Xiuli, SHAN Xiaomei
Received:
2020-05-29
Online:
2021-04-08
Published:
2021-03-08
Contact:
LIU Bolin
摘要:
建立了固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)同时检测鸡蛋、液态奶、鸡肉及淡水鱼中4类(氯霉素类、硝基咪唑类、林可酰胺类与大环内酯类)8种禁限兽药与3种代谢物残留的分析方法。对样品前处理及色谱条件进行优化,样品经0.1 mol/L pH 9.0的磷酸盐缓冲液水解分散,乙腈提取,提取液经乙酸乙酯萃取后浓缩至近干,残留物用0.3 mL甲醇溶解,再加入5.7 mL磷酸盐缓冲液,混匀,溶解液经Oasis HLB固相萃取柱净化后上机分析,以甲醇与0.1%甲酸水溶液作为流动相进行梯度洗脱,经ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm, 1.7 μm)分离,采用ESI+和ESI-电离,在多反应监测模式下采集,同位素内标法定量。结果表明,11种待测物在色谱柱上完全基线分离,在各自范围内线性关系良好,相关系数(R2)>0.99,方法的检出限(LOD)为0.050~0.50 μg/kg,定量限(LOQ)为0.20~1.5 μg/kg。各待测物的平均回收率为65.3%~108%,相对标准偏差(RSD)为0.40%~21%。将该方法应用于市售样品中上述4类兽药残留的常规监测,其阳性样本的检测结果与标准方法测定结果无显著性差异。该方法灵敏度高,稳定性好,定量准确,适用于动物源性食品中多种禁限兽药及代谢物残留的同时快速测定。
中图分类号:
刘柏林, 谢继安, 赵紫微, 王秀莉, 单晓梅. 固相萃取-超高效液相色谱-串联质谱法同时测定动物源性食品中11种禁限兽药及代谢物[J]. 色谱, 2021, 39(4): 406-414.
LIU Bolin, XIE Jian, ZHAO Ziwei, WANG Xiuli, SHAN Xiaomei. Simultaneous determination of 11 prohibited and restricted veterinary drugs and their metabolites in animal-derived foods by ultra performance liquid chromatography-tandem mass spectrometry coupled with solid phase extraction[J]. Chinese Journal of Chromatography, 2021, 39(4): 406-414.
Analyte | ESI | tR/ min | Parent ion (m/z) | Product ions (m/z) | Collision energies/eV | Cone voltage/ V | IS |
---|---|---|---|---|---|---|---|
Florfenicol amine (氟苯尼考胺) | + | 0.84 | 248.1 | 230.1*/130.1 | 12/24 | 30 | florfenicol amine-D3 |
Metronidazole (甲硝唑) | + | 1.49 | 172.1 | 128.1*/82.0 | 14/22 | 30 | metronidazole-D4 |
Ronidazole (洛硝达唑) | + | 1.55 | 201 | 140.0*/55.1 | 12/20 | 24 | ronidazole-D3 |
Dimetridazole (地美硝唑) | + | 1.68 | 142.1 | 96.0*/81.0 | 16/22 | 36 | dimetridazole-D3 |
Thiamphenicol (甲砜霉素) | - | 2.2 | 354 | 185.0*/290.1 | 20/12 | 30 | thiamphenicol-D3 |
Lincomycin (林可霉素) | + | 2.43 | 407.4 | 126.1*/359.3 | 28/20 | 52 | lincomycin-D3 |
Florfenicol (氟苯尼考) | - | 2.89 | 356 | 185.0*/336.1 | 18/10 | 36 | florfenicol-D3 |
Chloramphenicol (氯霉素) | - | 3.71 | 321 | 257.0/152.0* | 10/20 | 30 | chloramphenicol-D5 |
Erythromycin A (红霉素A) | + | 4.25 | 734.5 | 158.1*/576.5 | 28/20 | 48 | erythromycin A-D6 |
Erythromycin A enol ether | + | 4.28 | 716.4 | 158.1*/83.0/558.3 | 30/42/20 | 44 | erythromycin A-D6 |
(红霉素A烯醇醚) | |||||||
Anhydro erythromycin A (脱氧红霉素A) | + | 4.42 | 716.4 | 158.1*/558.3 | 30/16 | 38 | erythromycin A-D6 |
Florfenicol amine-D3 (氟苯尼考胺-D3) | + | 0.83 | 251.2 | 233.1*/130.2 | 12/24 | 30 | |
Metronidazole-D4 (甲硝唑-D4) | + | 1.49 | 176.2 | 128.1*/82.0 | 16/26 | 30 | |
Ronidazole-D3 (洛硝达唑-D3) | + | 1.55 | 204 | 143.0*/58.0 | 20/12 | 24 | |
Dimetridazole-D3 (地美硝唑-D3) | + | 1.68 | 145 | 99.0*/83.0 | 22/16 | 36 | |
Thiamphenicol-D3 (甲砜霉素-D3) | - | 2.2 | 357.1 | 188.1*/293.1 | 20/12 | 40 | |
Lincomycin-D3 (林可霉素-D3) | + | 2.43 | 410.4 | 129.1*/362.3 | 28/20 | 52 | |
Florfenicol-D3 (氟苯尼考-D3) | - | 2.89 | 359.1 | 188.1*/339.1 | 18/10 | 36 | |
Chloramphenicol-D5(氯霉素-D5) | - | 3.71 | 326 | 157.0*/262.0 | 18/12 | 30 | |
Erythromycin A-D6 (红霉素A-D6) | + | 4.25 | 740.5 | 164.1*/582.5 | 32/20 | 48 |
表 1 11种待测物及9种同位素内标的质谱参数
Table 1 MS parameters for the 11 analytes and 9 isotope internal standards
Analyte | ESI | tR/ min | Parent ion (m/z) | Product ions (m/z) | Collision energies/eV | Cone voltage/ V | IS |
---|---|---|---|---|---|---|---|
Florfenicol amine (氟苯尼考胺) | + | 0.84 | 248.1 | 230.1*/130.1 | 12/24 | 30 | florfenicol amine-D3 |
Metronidazole (甲硝唑) | + | 1.49 | 172.1 | 128.1*/82.0 | 14/22 | 30 | metronidazole-D4 |
Ronidazole (洛硝达唑) | + | 1.55 | 201 | 140.0*/55.1 | 12/20 | 24 | ronidazole-D3 |
Dimetridazole (地美硝唑) | + | 1.68 | 142.1 | 96.0*/81.0 | 16/22 | 36 | dimetridazole-D3 |
Thiamphenicol (甲砜霉素) | - | 2.2 | 354 | 185.0*/290.1 | 20/12 | 30 | thiamphenicol-D3 |
Lincomycin (林可霉素) | + | 2.43 | 407.4 | 126.1*/359.3 | 28/20 | 52 | lincomycin-D3 |
Florfenicol (氟苯尼考) | - | 2.89 | 356 | 185.0*/336.1 | 18/10 | 36 | florfenicol-D3 |
Chloramphenicol (氯霉素) | - | 3.71 | 321 | 257.0/152.0* | 10/20 | 30 | chloramphenicol-D5 |
Erythromycin A (红霉素A) | + | 4.25 | 734.5 | 158.1*/576.5 | 28/20 | 48 | erythromycin A-D6 |
Erythromycin A enol ether | + | 4.28 | 716.4 | 158.1*/83.0/558.3 | 30/42/20 | 44 | erythromycin A-D6 |
(红霉素A烯醇醚) | |||||||
Anhydro erythromycin A (脱氧红霉素A) | + | 4.42 | 716.4 | 158.1*/558.3 | 30/16 | 38 | erythromycin A-D6 |
Florfenicol amine-D3 (氟苯尼考胺-D3) | + | 0.83 | 251.2 | 233.1*/130.2 | 12/24 | 30 | |
Metronidazole-D4 (甲硝唑-D4) | + | 1.49 | 176.2 | 128.1*/82.0 | 16/26 | 30 | |
Ronidazole-D3 (洛硝达唑-D3) | + | 1.55 | 204 | 143.0*/58.0 | 20/12 | 24 | |
Dimetridazole-D3 (地美硝唑-D3) | + | 1.68 | 145 | 99.0*/83.0 | 22/16 | 36 | |
Thiamphenicol-D3 (甲砜霉素-D3) | - | 2.2 | 357.1 | 188.1*/293.1 | 20/12 | 40 | |
Lincomycin-D3 (林可霉素-D3) | + | 2.43 | 410.4 | 129.1*/362.3 | 28/20 | 52 | |
Florfenicol-D3 (氟苯尼考-D3) | - | 2.89 | 359.1 | 188.1*/339.1 | 18/10 | 36 | |
Chloramphenicol-D5(氯霉素-D5) | - | 3.71 | 326 | 157.0*/262.0 | 18/12 | 30 | |
Erythromycin A-D6 (红霉素A-D6) | + | 4.25 | 740.5 | 164.1*/582.5 | 32/20 | 48 |
图 1 11种禁限兽药及代谢物的总离子流色谱图
Fig. 1 Total ion current (TIC)chromatograms of the 11 prohibited and restricted veterinary drugs and their metabolites 1. florfenicol amine; 2. metronidazole; 3. ronidazole; 4. dimetridazole; 5. thiamphenicol; 6. lincomycin; 7. florfenicol; 8. chloramphenicol; 9. erythromycin A; 10. erythromycin A enol ether; 11. anhydro erythromycin A.
图 2 磷酸盐缓冲液的pH值对11种禁限兽药及代谢物提取效率的影响
Fig. 2 Effect of different phosphate buffer pH values on the extraction efficiencies of the 11 prohibited and restricted veterinary drugs and their metabolites
图 3 不同净化方式对11种禁限兽药及代谢物回收率的影响(n=3)
Fig. 3 Effect of different purification methods on the recoveries of the 11 prohibited and restricted veterinary drugs and their metabolites (n=3)
Analyte | Linear equation | Linear range/(μg/L) | R2 | LOD/(μg/kg) | LOQ/(μg/kg) |
---|---|---|---|---|---|
Florfenicol amine | y=0.0898x-0.0035 | 0.1-50 | 0.9992 | 0.050 | 0.20 |
Metronidazole | y=0.1920x-0.0171 | 0.1-50 | 0.9972 | 0.050 | 0.20 |
Ronidazole | y=0.1535x-0.0172 | 0.1-50 | 0.9982 | 0.050 | 0.20 |
Dimetridazole | y=0.1894x-0.0155 | 0.1-50 | 0.9968 | 0.050 | 0.20 |
Thiamphenicol | y=0.0949x-0.0163 | 1.0-50 | 0.9927 | 0.50 | 1.5 |
Lincomycin | y=0.1311x-0.0088 | 0.1-50 | 0.9988 | 0.050 | 0.20 |
Florfenicol | y=0.0756x+0.0049 | 0.5-50 | 0.9971 | 0.25 | 0.80 |
Chloramphenicol | y=0.2078x+0.0066 | 0.5-50 | 0.9981 | 0.25 | 0.80 |
Erythromycin A | y=0.1283x-0.0116 | 0.2-50 | 0.9991 | 0.10 | 0.30 |
Erythromycin A enol ether | y=0.0705x-0.0099 | 0.2-50 | 0.9969 | 0.10 | 0.30 |
Anhydro erythromycin A | y=0.1414x-0.0336 | 0.2-50 | 0.9914 | 0.10 | 0.30 |
表 2 11种禁限兽药及代谢物的线性方程、线性范围、相关系数、检出限和定量限
Table 2 Linear equations, linear ranges, correlation coefficients (R2), LODs, and LOQs for the 11 prohibited and restricted veterinary drugs and their metabolites
Analyte | Linear equation | Linear range/(μg/L) | R2 | LOD/(μg/kg) | LOQ/(μg/kg) |
---|---|---|---|---|---|
Florfenicol amine | y=0.0898x-0.0035 | 0.1-50 | 0.9992 | 0.050 | 0.20 |
Metronidazole | y=0.1920x-0.0171 | 0.1-50 | 0.9972 | 0.050 | 0.20 |
Ronidazole | y=0.1535x-0.0172 | 0.1-50 | 0.9982 | 0.050 | 0.20 |
Dimetridazole | y=0.1894x-0.0155 | 0.1-50 | 0.9968 | 0.050 | 0.20 |
Thiamphenicol | y=0.0949x-0.0163 | 1.0-50 | 0.9927 | 0.50 | 1.5 |
Lincomycin | y=0.1311x-0.0088 | 0.1-50 | 0.9988 | 0.050 | 0.20 |
Florfenicol | y=0.0756x+0.0049 | 0.5-50 | 0.9971 | 0.25 | 0.80 |
Chloramphenicol | y=0.2078x+0.0066 | 0.5-50 | 0.9981 | 0.25 | 0.80 |
Erythromycin A | y=0.1283x-0.0116 | 0.2-50 | 0.9991 | 0.10 | 0.30 |
Erythromycin A enol ether | y=0.0705x-0.0099 | 0.2-50 | 0.9969 | 0.10 | 0.30 |
Anhydro erythromycin A | y=0.1414x-0.0336 | 0.2-50 | 0.9914 | 0.10 | 0.30 |
Analyte | Spiked level/ (μg/kg) | Recoveries/% | RSDs/% | ||||||||
---|---|---|---|---|---|---|---|---|---|---|---|
Egg | Fish | Chicken | Milk | Egg | Fish | Chicken | Milk | ||||
Florfenicol amine | 0.2 | 97.9 | 89.7 | 98.4 | 94.0 | 11 | 13 | 10 | 14 | ||
2.0 | 93.4 | 92.9 | 94.5 | 92.5 | 1.4 | 2.2 | 6.2 | 7.2 | |||
100 | 97.1 | 100 | 94.0 | 92.3 | 6.8 | 2.4 | 11 | 4.9 | |||
Metronidazole | 0.2 | 92.5 | 84.1 | 84.1 | 86.3 | 2.0 | 3.7 | 2.7 | 3.1 | ||
2.0 | 91.0 | 83.8 | 77.9 | 81.5 | 3.3 | 1.5 | 1.1 | 3.3 | |||
20 | 98.2 | 95.9 | 107 | 103 | 5.3 | 6.3 | 2.2 | 3.3 | |||
Ronidazole | 0.2 | 92.5 | 95.4 | 98.7 | 93.7 | 4.5 | 5.0 | 2.8 | 6.8 | ||
2.0 | 96.2 | 95.3 | 95.8 | 93.6 | 2.0 | 2.9 | 2.0 | 4.8 | |||
20 | 94.4 | 93.5 | 107 | 94.8 | 1.7 | 1.9 | 4.0 | 7.3 | |||
Dimetridazole | 0.2 | 99.0 | 105 | 100 | 102 | 7.8 | 2.8 | 2.1 | 5.1 | ||
2.0 | 100 | 98.2 | 94.0 | 97.3 | 2.1 | 4.8 | 1.4 | 3.6 | |||
20 | 96.5 | 97.7 | 83.8 | 104 | 6.7 | 7.2 | 5.2 | 6.9 | |||
Thiamphenicol | 2.0 | 95.0 | 99.8 | 97.7 | 98.4 | 6.2 | 2.8 | 1.6 | 4.6 | ||
10 | 102 | 97.4 | 101 | 103 | 0.40 | 1.2 | 2.7 | 2.4 | |||
50 | 98.0 | 98.8 | 98.4 | 98.6 | 7.0 | 8.9 | 5.8 | 2.8 | |||
Lincomycin | 0.2 | 102 | 91.9 | 89.7 | 85.8 | 6.2 | 9.9 | 4.1 | 3.3 | ||
2.0 | 97.5 | 91.0 | 94.3 | 90.5 | 5.0 | 3.9 | 5.6 | 0.94 | |||
50 | 83.6 | 76.7 | 77.8 | 95.0 | 1.5 | 5.4 | 10 | 8.6 | |||
Florfenicol | 1.0 | 98.6 | 100 | 101 | 100 | 6.9 | 9.6 | 11 | 10 | ||
2.0 | 102 | 99.1 | 99.5 | 98.3 | 2.5 | 2.07 | 2.90 | 3.3 | |||
100 | 104 | 103 | 101 | 100 | 2.4 | 1.2 | 5.3 | 4.4 | |||
Chloramphenicol | 1.0 | 102 | 107 | 108 | 106 | 3.4 | 2.0 | 1.7 | 0.76 | ||
2.0 | 101 | 99.5 | 103 | 102 | 0.55 | 3.2 | 3.1 | 4.2 | |||
10 | 103 | 101 | 103 | 107 | 5.3 | 3.0 | 4.2 | 2.0 | |||
Erythromycin A | 0.3 | 87.5 | 93.5 | 90.7 | 94.7 | 4.7 | 4.2 | 1.1 | 5.5 | ||
2.0 | 86.4 | 93.9 | 92.1 | 93.7 | 0.88 | 2.1 | 4.2 | 5.2 | |||
40 | 104 | 102 | 100 | 99.7 | 5.5 | 0.8 | 4.2 | 5.6 | |||
Erythromycin A enol ether | 0.3 | 65.3 | 104 | 84.4 | 82.1 | 11 | 4.2 | 15 | 8.1 | ||
2.0 | 76.1 | 97.2 | 71.2 | 90.2 | 13 | 4.2 | 21 | 11 | |||
10 | 86.9 | 99.9 | 83.2 | 90.2 | 14 | 3.9 | 10 | 7.0 | |||
Anhydro erythromycin A | 0.3 | 101 | 86.3 | 98.7 | 94.4 | 2.7 | 5.5 | 9.3 | 6.0 | ||
2.0 | 105 | 94.6 | 96.6 | 98.8 | 0.44 | 12 | 6.2 | 7.4 | |||
10 | 105 | 95.0 | 102 | 108 | 8.8 | 16 | 4.4 | 0.85 |
表 3 11种禁限兽药及代谢物在实际样品中的加标回收率和相对标准偏差(n=6)
Table 3 Spiked recoveries and RSDs of the 11 prohibited and restricted veterinary drugs and their metabolites in real samples (n=6)
Analyte | Spiked level/ (μg/kg) | Recoveries/% | RSDs/% | ||||||||
---|---|---|---|---|---|---|---|---|---|---|---|
Egg | Fish | Chicken | Milk | Egg | Fish | Chicken | Milk | ||||
Florfenicol amine | 0.2 | 97.9 | 89.7 | 98.4 | 94.0 | 11 | 13 | 10 | 14 | ||
2.0 | 93.4 | 92.9 | 94.5 | 92.5 | 1.4 | 2.2 | 6.2 | 7.2 | |||
100 | 97.1 | 100 | 94.0 | 92.3 | 6.8 | 2.4 | 11 | 4.9 | |||
Metronidazole | 0.2 | 92.5 | 84.1 | 84.1 | 86.3 | 2.0 | 3.7 | 2.7 | 3.1 | ||
2.0 | 91.0 | 83.8 | 77.9 | 81.5 | 3.3 | 1.5 | 1.1 | 3.3 | |||
20 | 98.2 | 95.9 | 107 | 103 | 5.3 | 6.3 | 2.2 | 3.3 | |||
Ronidazole | 0.2 | 92.5 | 95.4 | 98.7 | 93.7 | 4.5 | 5.0 | 2.8 | 6.8 | ||
2.0 | 96.2 | 95.3 | 95.8 | 93.6 | 2.0 | 2.9 | 2.0 | 4.8 | |||
20 | 94.4 | 93.5 | 107 | 94.8 | 1.7 | 1.9 | 4.0 | 7.3 | |||
Dimetridazole | 0.2 | 99.0 | 105 | 100 | 102 | 7.8 | 2.8 | 2.1 | 5.1 | ||
2.0 | 100 | 98.2 | 94.0 | 97.3 | 2.1 | 4.8 | 1.4 | 3.6 | |||
20 | 96.5 | 97.7 | 83.8 | 104 | 6.7 | 7.2 | 5.2 | 6.9 | |||
Thiamphenicol | 2.0 | 95.0 | 99.8 | 97.7 | 98.4 | 6.2 | 2.8 | 1.6 | 4.6 | ||
10 | 102 | 97.4 | 101 | 103 | 0.40 | 1.2 | 2.7 | 2.4 | |||
50 | 98.0 | 98.8 | 98.4 | 98.6 | 7.0 | 8.9 | 5.8 | 2.8 | |||
Lincomycin | 0.2 | 102 | 91.9 | 89.7 | 85.8 | 6.2 | 9.9 | 4.1 | 3.3 | ||
2.0 | 97.5 | 91.0 | 94.3 | 90.5 | 5.0 | 3.9 | 5.6 | 0.94 | |||
50 | 83.6 | 76.7 | 77.8 | 95.0 | 1.5 | 5.4 | 10 | 8.6 | |||
Florfenicol | 1.0 | 98.6 | 100 | 101 | 100 | 6.9 | 9.6 | 11 | 10 | ||
2.0 | 102 | 99.1 | 99.5 | 98.3 | 2.5 | 2.07 | 2.90 | 3.3 | |||
100 | 104 | 103 | 101 | 100 | 2.4 | 1.2 | 5.3 | 4.4 | |||
Chloramphenicol | 1.0 | 102 | 107 | 108 | 106 | 3.4 | 2.0 | 1.7 | 0.76 | ||
2.0 | 101 | 99.5 | 103 | 102 | 0.55 | 3.2 | 3.1 | 4.2 | |||
10 | 103 | 101 | 103 | 107 | 5.3 | 3.0 | 4.2 | 2.0 | |||
Erythromycin A | 0.3 | 87.5 | 93.5 | 90.7 | 94.7 | 4.7 | 4.2 | 1.1 | 5.5 | ||
2.0 | 86.4 | 93.9 | 92.1 | 93.7 | 0.88 | 2.1 | 4.2 | 5.2 | |||
40 | 104 | 102 | 100 | 99.7 | 5.5 | 0.8 | 4.2 | 5.6 | |||
Erythromycin A enol ether | 0.3 | 65.3 | 104 | 84.4 | 82.1 | 11 | 4.2 | 15 | 8.1 | ||
2.0 | 76.1 | 97.2 | 71.2 | 90.2 | 13 | 4.2 | 21 | 11 | |||
10 | 86.9 | 99.9 | 83.2 | 90.2 | 14 | 3.9 | 10 | 7.0 | |||
Anhydro erythromycin A | 0.3 | 101 | 86.3 | 98.7 | 94.4 | 2.7 | 5.5 | 9.3 | 6.0 | ||
2.0 | 105 | 94.6 | 96.6 | 98.8 | 0.44 | 12 | 6.2 | 7.4 | |||
10 | 105 | 95.0 | 102 | 108 | 8.8 | 16 | 4.4 | 0.85 |
[1] | Ke Q Q, Li S Y, Zhou F, et al. Food Science, 2017,38(24):241 |
柯庆青, 李诗言, 周凡, 等. 食品科学, 2017,38(24):241 | |
[2] |
Hou J B, Xie W, Chen X M, et al. Chinese Journal of Chromatography, 2011,29(6):535
DOI URL |
侯建波, 谢文, 陈笑梅, 等. 色谱, 2011,29(6):535
DOI URL |
|
[3] | Zhang X Y, Zheng D Z, Yuan F, et al. Journal of Instrumental Analysis, 2013,32(9):1131 |
张晓燕, 郑定钊, 袁芳, 等. 分析测试学报, 2013,32(9):1131 | |
[4] | Zhang X Y, Zhang X Y, Cai X X, et al. Preventive Medicine, 2019,31(2):212 |
张晓艺, 张秀尧, 蔡欣欣, 等. 预防医学, 2019,31(2):212 | |
[5] | Meng Z, Shi Z H, Lü Y K, et al. Chinese Journal of Analytical Chemistry, 2014,42(10):1493 |
孟哲, 石志红, 吕运开, 等. 分析化学, 2014,42(10):1493 | |
[6] | Gong S S, Zhang J, Yan F, et al. Journal of Instrumental Analysis, 2019,38(1):22 |
贡松松, 张婧, 严凤, 等. 分析测试学报, 2019,38(1):22 | |
[7] |
Li R, Yang L Q, Zhang P Y, et al. Chinese Journal of Chromatography, 2017,35(12):1266
DOI URL PMID |
李蓉, 杨璐齐, 张鹏云, 等. 色谱, 2017,35(12):1266
PMID |
|
[8] | Cheng J, Zhao S Z, Huo Y H, et al. Journal of Food Safety and Quality, 2018,9(3):574 |
程甲, 赵善贞, 霍忆慧, 等. 食品安全质量检测学报, 2018,9(3):574 | |
[9] |
Li S, Chen S B, Li L Q, et al. Chinese Journal of Chromatography, 2018,36(6):506
DOI URL PMID |
李双, 陈树兵, 李露青, 等. 色谱, 2018,36(6):506
PMID |
|
[10] | Zhang C W, Wu Z M, Li H C, et al. Journal of Instrumental Analysis, 2020,39(2):174 |
张崇威, 吴志明, 李华岑, 等. 分析测试学报, 2020,39(2):174 | |
[11] | Fang L, Wei H, Huang B, et al. Journal of Instrumental Analysis, 2019,38(6):681 |
方灵, 韦航, 黄彪, 等. 分析测试学报, 2019,38(6):681 | |
[12] |
Wang H, Zhao L, Yang H M, et al. Chinese Journal of Chromatography, 2015,33(9):995
DOI URL |
王浩, 赵丽, 杨红梅, 等. 色谱, 2015,33(9):995
DOI URL |
|
[13] | Zeng Y, Dong W T, Gong B, et al. Chinese Journal of Veterinary Drug, 2017,51(12):42 |
曾勇, 董文婷, 龚波, 等. 中国兽药杂志, 2017,51(12):42 | |
[14] | Yan Z Y, Zhang X J, Li P P, et al. Journal of Zhejiang University (Science Edition), 2017,44(3):339 |
严忠雍, 张小军, 李佩佩, 等. 浙江大学学报(理学版), 2017,44(3):339 | |
[15] |
Wittenberg J B, Simon K A, Wong J W. J Agric Food Chem, 2017,65(34):7288
DOI URL PMID |
[16] | Jiang D Z, Xin L N, Tan X M, et al. Science and Technology of Food Industry, 2019,40(22):259 |
蒋定之, 辛丽娜, 谭喜梅, 等. 食品工业科技, 2019,40(22):259 | |
[17] |
Chen X L, Lin T, Liu X Y, et al. Chinese Journal of Chromatography, 2019,37(9):946
DOI URL PMID |
陈兴连, 林涛, 刘兴勇, 等. 色谱, 2019,37(9):946
PMID |
|
[18] | Chen X L, Lin T, Liu X Y, et al. Chinese Journal of Chromatography, 2020,38(5):538 |
陈兴连, 林涛, 刘兴勇, 等. 色谱, 2020,38(5):538 | |
[19] |
Gibbs R S, Murray S L, Watson L V, et al. J Agric Food Chem, 2018,66(20):4997
DOI URL PMID |
[20] | Chorghade M S. Drug Discovery and Development, Volume 1. Hoboken: John Wiley & Sons, Inc., 2006 |
[21] | Yang D J, Li N. Manual for China National Food Contamination and Harmful Factors Risk Monitoring. Beijing: Standards Press of China, 2014 |
杨大进, 李宁. 国家食品污染物和有害因素监测工作手册. 北京: 中国标准出版社, 2014 | |
[22] |
Kwon H, Lehotay S J, Geis-Asteggiante L. J Chromatogr A, 2012,1270:235
DOI URL |
[23] |
Besil N, Cesio V, Heinzen H, et al. J Agric Food Chem, 2017,65(23):4819
DOI URL PMID |
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