Determination of 56 drug residues in milk powder by high performance liquid chromatography-tandem mass spectrometry in multiple reaction monitoring mode

  • ZHOU Chunhong ,
  • XU Xiaohui
Expand
  • 1(GanSu Province Product Quality Supervision and Inspection Research Institute, Lanzhou 730000, China)
    2(Lanzhou Institute for Food and Drug Control, Lanzhou 730000, China)

Received date: 2021-03-22

  Revised date: 2021-05-31

  Online published: 2021-10-18

Abstract

A high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) was established for the simultaneous analysis of 56 drug residues in milk powder. Each sample was dissolved in water and extracted with acidified acetonitrile, then purified with QuEchERS, and finally detected by LC-MS/MS with electrospray ionization in multiple reaction monitoring mode. Some compounds were quantified by the external standard method. The results showed that there were good linear relationships for 56 drugs with correlation coefficients not less than 0.999. The detection limits and quantification for 56 drug residues were 0.06-5.47 and 0.21-16.53 μg/kg respectively. The average recoveries at three spiked levels of 2, 5 and 10 μg/kg were in the range of 61.3%-129.8% which with relative standard deviations (RSD) of 0.090%-7.171% (n=6). Thus, the optimized method is rapid, simple and easy. And it can be widely used in the rapid screening and quantitative detection of multiple drug residues in adult milk powder.

Cite this article

ZHOU Chunhong , XU Xiaohui . Determination of 56 drug residues in milk powder by high performance liquid chromatography-tandem mass spectrometry in multiple reaction monitoring mode[J]. Food and Fermentation Industries, 2021 , 47(18) : 250 -257 . DOI: 10.13995/j.cnki.11-1802/ts.027385

References

[1] 黑真真. 风险物质快速筛查在食品安全检测中的应用研究[D].北京:中国食品药品检定研究院, 2019.
HEI Z Z.Study on the application of rapid screening of risk substances in food safety detection[D].Beijing:National Institutes for Food and Drug Control, 2019.
[2] 李红丽. QuEChERS-UPLC-MS/MS同时测定动物性食品中24种残留兽药方法及基质效应的研究[D].重庆:西南大学, 2020.
LI H L.Study on simultaneous determination of 24 veterinary drug residues contained in animal derived foods and the matrix effect with QuEChERS-UPLC-MS/MS[D].Chongqing:Southwest University, 2020.
[3] 陈兴连, 林涛, 刘兴勇, 等.超高效液相色谱-串联质谱法快速测定鱼和虾中多类禁、限用兽药残留[J].色谱, 2020, 38(5):538-546.
CHENG X L, LIN T, LIU X Y, et al.Rapid determination of multiple prohibited and restricted veterinary drug residues in fish and shrimp by ultra high performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography, 2020, 38(5):538-546.
[4] 李芹. QuEChERS技术在水产品中利福平和12种镇静剂残留检测中的应用[D].上海:上海海洋大学, 2020.
LI Q.Application of QuEChERS technology in the detection of rifampicin and 12 Kinds of sedatives residues in aquatic products[D].Shanghai:Shanghai Ocean University, 2020.
[5] ÁLVAREZ-FREIRE I, BRUNETTI P, CABARCOS-FERNÁNDEZ P, et al.Determination of benzodiazepines in pericardial fluid by gas chromatography-mass spectrometry[J].Journal of Pharmaceutical and Biomedical Analysis, 2018, 159:45-52.
[6] 黄越燕, 屠婕红, 徐宏祥, 等.UPLC-MS/MS法快速测定中药及保健食品中非法添加17种抗炎镇痛类化学药的研究[J].中草药, 2016, 47(2):246-254.
HUANG Y Y, TU J H, XU H X, et al.Rapid determination of 17 anti-inflammatory and analgesic chemical illegally added into Chinese patent medicine and health foods by UPLC-MS/MS[J].Chinese traditional and Herbal Drugs, 2016, 47(2):246-254.
[7] 陈晓红, 林梦, 金米聪.生物样品中镇静类药物检测的研究进展[J].理化检验 (化学分册), 2020, 56(5):612-620.
CHEN X H, LIN M, JIN M C.Research progress on detection of sedative drugs in biological samples[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis), 2020, 56(5):612-620.
[8] AO J J, YUAN T, MA Y N, et al.Identification, characteristics and human exposure assessments of triclosan, bisphenol-A, and four commonly used organic UV filters in indoor dust collected from Shanghai, China[J].Chemosphere, 2017, 184:575-583.
[9] 冯雪伊, 陈航, 沈敏, 等.微波辅助提取/液相色谱-串联质谱法同时测定人体指甲中14种抗精神失常及安眠镇静类物质[J].分析测试学报, 2016, 35(10):1 233-1 240.
FENG X Y, CHEN H, SHEN M, et al.Simultaneous determinationof 14 antipsychotic and sedative substances in human nails using microwave-assisted extraction combined with liquid chromatography-tandem mass spectrometry[J].Journal of Instrumental Analysis, 2016, 35(10):1 233-1 240.
[10] SIM J, KIM E, YANG W, et al.An LC-MS/MS method for the simultaneous determination of 15 antipsychotics and two metabolites in hair and its application to rat hair[J].Forensic Science International, 2017, 274:91-98.
[11] JUNIOR E F, CALDAS E D.Simultaneous determination of drugs and pesticides in postmortem blood using dispersive solid-phese extraction and large volume injection-programmed temperature vaporization-gas chromatography-mass spectrometry[J].Forensic Science International, 2018, 290:318-326.
[12] 段筱筠. 动物源性食品中磺胺类药物残留检测的绿色高效液相色谱方法研究[D].兰州:兰州理工大学, 2020.
DUAN X Y.Study on the green high performance liquid chromatographic methods for detection of sulfonamides residues in animal derived foods[D].Lanzhou:Lanzhou University of Technology, 2020.
[13] 金晓峰, 焦仁刚, 赵贵, 等.通过式固相萃取/超高效液相色谱-串联质谱法快速测定鸡蛋中的8种兽药残留[J].分析科学学报, 2020, 36(6):906-911.
JIN X F, JIAO R G, ZHAO G, et al.Determination of eight veterinary drugs in eggs by ultra-high performance liquid chromatography-tandem mass spectrometry with a through-type solid-phase extraction[J].Journal of Analytical Science, 2020, 36(6):906-911.
[14] 方灵, 韦航, 黄彪, 等.超高效液相色谱-串联质谱法同时测定牛奶中38种抗生素残留[J].分析测试学报, 2019, 38(6):681-686;692.
FANG L, WEI H, HUANG B, et al.Simultaneous determination of 38 antibiotics residues in milk by ultra-high performance liquid chromatography-tandem mass spectrometry[J].Journal of Instrumental Analysis, 2019, 38(6):681-686;692.
[15] 王卉, 刘庆菊, 韩平.超高效液相色谱-串联质谱法测定牛奶中23种兽药[J].食品工业, 2020, 41(8):312-317.
WANG H, LIU Q J, HAN P.Determination of 23 veterinary drugs in milk by ultra-high performance liquid chromatography-tandem mass spectrometry method[J].The Food Industry, 2020, 41(8):312-317.
[16] KHELFI A, AZZOUZ M, ABTROUN R, et al.Determination of chlorpromazine, haloperidol, levomepromazine, olanzapine, risperidone, and sulpiride in human plasma by liquid chromatography/tandem mass spectrometry (LC-MS/MS)[J].International Journal of Analytical Chemistry, 2018.DOI:10.1155/2018/5807218.
[17] PETTERSSON BERGSTRAND M, BECK O, HELANDER A.Urine analysis of 28 designer benzodiazepines by liquid chromatography-high-resolution mass spectrometry[J].Clinical Mass Spectrometry, 2018, 10:25-32.
[18] 张崇威, 吴志明, 李华岑, 等.Captiva EMR-Lipid固相萃取/超高效液相色谱-串联质谱法快速筛查动物源食品中51种药物残留[J].分析测试学报, 2020, 39(2):174-181.
ZHANG C W, WU Z M, LI H C, et al.Rapid screening of 51 drug residues in animal products by captiva EMR-lipid solid phase extraction/ultra-high performance liquid chromatography-tandem mass spectrometry[J].Journal of Instrumental Analysis, 2020, 39(2):174-181.
[19] 陈兴连, 林涛, 刘兴勇, 等.分散固相萃取净化-超高效液相色谱-串联质谱法同时测定鱼和虾中抗生素及三苯甲烷类兽药残留[J].色谱, 2019, 37(9):946-954.
CHEN X L, LIN T, LIU X Y, et al.Simultaneous determination of antibiotics and triphenylmethanes veterinary drug residues in fish and shrimp by dispersive solid phase extraction purification-ultra high performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography, 2019, 37(9):946-954.
[20] 刘家阳, 黄旭, 贾宏新.固相萃取/超高效液相色谱-串联质谱法测定畜肉中16种镇静剂类兽药留[J].分析测试学报, 2017, 36(3):305-311.
LIU J Y, HUANG X, JIA H X.Simultaneous determination of 16 sedative residues in livestock products by solid phase extraction/ultra performance liquid chromatography-tandem mass spectrometry[J].Journal of Instrumental Analysis, 2017, 36(3):305-311.
[21] 徐迪, 马康, 单吉浩, 等.超高效液相色谱-串联质谱法测定动物尿液中5种镇静剂类药物残留[J].核农学报, 2020, 34(9):2 045-2 050.
XU D, MA K, SHAN J H, et al.Determination of five sedative drug residues in animal urine by ultra high performance liquid chromatography-tandem mass spectrometry[J].Journal of Nuclear Agricultural Sciences, 2020, 34(9):2 045-2 050.
[22] 钱卓真, 汤水粉, 梁焱, 等.QuEChERS-高效液相色谱-串联质谱法同时测定水产养殖环境沉积物中磺胺类、喹诺酮类、大环内酯类抗生素[J].质谱学报, 2019, 40(4):356-368.
QIAN Z Z, TANG S F, LIANG Y, et al.Simultaneous determination of sulfonamides, quinolones and macrolides antibiotics residues in sediment from aquaculture environment by QuEChERS-HPLC-MS/MS[J].Journal of Chinese Mass Spectrometry Society, 2019, 40(4):356-368.
[23] 刘权辉, 王彤彤, 王敏, 等.QuEChERS在动物源食品药物残留前处理方法的进展[J].化学试剂, 2020, 42(12):1 424-1 429.
LIU Q H, WANG T T, WANG M, et al.Progress of QuEChERS in pretreatment method of drug residues in animal-derived foods[J].Chemical Reagents, 2020, 42(12):1 424-1 429.
Outlines

/