通过式固相萃取-液相色谱-串联质谱法测定食品中的氯米芬、曲美他嗪和美度铵

摘要/Abstract

摘要： 建立通过式固相萃取-液相色谱-串联质谱法测定食品中的曲美他嗪、氯米芬和美度铵残留量的方法。样品采用5%甲酸乙腈提取，固相萃取小柱净化，经Amide色谱柱（3.0 mm×100 mm，1.7 μm）分离后，在多反应监测模式下测定，内标法定量。氯米芬和曲美他嗪在1.0～40.0 ng/mL质量浓度范围内线性关系良好；美度铵在5.0～200.0 ng/mL质量浓度范围内线性关系良好。测定结果相对标准偏差为0.3%～6.1%（n=6），平均加标回收率为81.3%～100.7%。该方法简便快速，实用性强，普遍适用于食品中的氯米芬、曲美他嗪和美度铵的测定，可为体育赛事的食品保障工作提供有效的技术支撑。

关键词: 氯米芬, 曲美他嗪, 美度铵, 超高效液相色谱-串联质谱法, 固相萃取

Abstract: In this study, we established a method for the determination of three metabolic regulators in foods by pass-through solid phase extraction-high performance liquid chromatography-tandem mass spectrometry (SPE-HPLC-MS/MS). The sample was extracted with 5% formic acid in acetonitrile, and the extract was purified by pass-through solid phase extraction column and passed through an amide(3.0 mm × 100 mm，1.7 μm) chromatography column .After separation, it was detected in the multiple reaction monitoring (MRM) mode, and quantitated by an internal standard method.The linear relationship between clomiphene and trimetazidine was good within the concentration range of 1.0~40.0 ng/mL; The linear relationship of meldonium was good within the concentration range of 5.0-200.0 ng/mL. The average recoveries ranged from 81.3% to 100.7%, and the relative standard deviations were between 0.3% and 6.1% (n=6). The developed method is simple, rapid and practical, and is suitable for the determination of the residues of three metabolic regulators in foods. It can provide effective technical support for the detection of foodborne stimulant drug residues.

Key words: clomiphene, trimetazidine, meldonium, high performance liquid chromatography-tandem mass spectrometry, solid phase extraction

中图分类号:

宋娟张阳阳李君姚蕾珺肖全伟李绍波戴琴. 通过式固相萃取-液相色谱-串联质谱法测定食品中的氯米芬、曲美他嗪和美度铵[J]. 食品科学.

君李蕾珺姚. Simultaneous Determination of 3 Metabolic Regulators Residues in Foods by high Performance Liquid Chromatography-Tandem Mass Spectrometry with pass-through solid phase extraction[J]. FOOD SCIENCE.

参考文献

[1] Sakar M N,Olak S C. The letrozole is superior to clomiphene citrate in ovulation induction in patients with polycystic ovary syndrome[J]. Pakistan Journal of Medical Sciences Online, 2020, 36(7): 1460-1465.
[2] Maheshwari A，Saraswat H，Upadhyay S K. Structural insights into the inclusion complexes between clomiphene citrate and β-cyclodextrin: The mechanism of preferential isomeric selection[J]. Chirality, 2017, 29(8): 451–457..
[3] Li, Qu, Hua, et al..Clinical efficacy of trimetazidine and holistic management in the treatment of coronary heart diseas[J]. Iran J Public Health, 2018, 47(6): 824-829．
[4] 郑锌,王雨晴,李莹, 等.亲水作用色谱-三重四极杆质谱法分析肉中代谢调节剂美度铵残留[J]. 环境化学, 2022(004): 1457-1460.
[5] 李佩濂, 姬文英. 高效液相色谱法测定枸橼酸氯米芬片中枸橼酸氯米芬[J]. 化学分析计量, 2021, 30(12): 47-50.
[6] 战余铭, 赵明晓, 朱良智, 等. 高效液相色谱法测定配合饲料中氯米芬的含量[J]. 中国农业科技导报, 2008, 10(S2): 48-52.
[7] 胡玉钦, 张运好, 蔡大伟, 等. 高效液相色谱-质谱联用测定人血浆中盐酸曲美他嗪[J]. 药物分析杂志, 2008, 28(7): 1050-1052.
[8] 曹国颖, 吕允凤, 胡欣, 等. 高效液相色谱-蒸发光散射检测法测定米屈肼中有关物质及含量[J]. 中国药学杂志, 2005, 40(11): 864-866.
[9] Peng Y , Jing Y , Wang Z R , et al. Determination of mildronate by LC-MS/MS and its application to a pharmacokinetic study in healthy Chinese volunteers.[J]. Journal of Chromatography B Analytical Technologies in the Biomedical & Life Sciences, 2010, 878(5-6): 551-556.
[10]Kim Y , Jeong D , Min H , et al. Method for screening and confirming meldonium in human urine by high-resolution mass spectrometry and identification of endogenous interferences for anti-doping testing[J]. Mass Spectrometry Letters, 2017, 8(2): 39-43.
[11]钟晓华. UPLC-MS/MS法同时检测人血浆中美托洛尔和曲美他嗪浓度[J]. 中国药师, 2022, 25(1): 178-182.
[12]Xhaferaj E, Naegele E, Parr M K. Ion exchange in supercritical fluid chromatography tandem mass spectrometry (SFCMS/MS): Application for polar and ionic drugs and metabolites in forensic and anti-doping analysis [J]. Journal of Chromatography A, 2020, 1614: 460726.
[13]许小友, 高平, 李洪波. 超高效液相色谱-串联质谱法测定鸡蛋中氯霉素的两种前处理方法比较[J]. 畜牧与兽医, 2019, 51(7): 51-54.
[14]Lu Z, Deng F, He R, et al. A pass-through solid-phase extraction clean-up method for the determination of 11 quinolone antibiotics in chicken meat and egg samples using ultra-performance liquid chromatography tandem mass spectrometry[J]. Microchemical Journal, 2019, 151: 104213.
[15]郭添荣, 万渝平, 孙利, 等. 通过式固相萃取结合超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查畜禽肉中108种兽药残留[J]. 分析化学, 2022, 50(02):271-289.
[16] 李道霞, 黄丽娟, 辜慧, 等. HPLC-MS/MS法检测动物源性食品中喹诺酮类药物的基质效应及其补偿措施研究[J]. 中国食品卫生杂志, 2022, 34(04): 693-699.
[17] CORTESE M, GIGLIOBIANCO M R, MAGNONI F, et al. Compensate for or minimize matrix effects? Strategies for overcoming matrix effects in liquid chromatography-mass spectrometry technique: a tutorial review[J]. Molecules, 2020, 25(13): 3047.
[18] 国家质量监督检验检疫总局, 国家标准化管理委员会. 实验室质量控制规范食品理化检测: GB/T 27404—2008[S]. 北京: 中国标准出版社, 2008: 1-33.