高效液相色谱-串联质谱法同时测定减肥类保健食品中27种违法添加化学药品
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摘要
目的:建立一种高效液相色谱-串联质谱(HPLC-MS/MS)同时测定减肥类保健食品中27种违法添加化学药品的方法。方法:采用Agilent Eclipse Plus C_(18)色谱柱(2.1 mm×100 mm,1.8μm),以10 mmol/L乙酸铵(用甲酸调节pH至4.0)溶液为流动相A,乙腈为流动相B,梯度洗脱,流速为0.2 m L/min。通过HPLC-MS/MS系统中多反应监测模式(MRM)对减肥类保健食品中27种违法添加化学药品进行定性和定量分析。结果:该方法线性R~2均大于0.99,精密度相对标准偏差小于8.0%,不同质量浓度样品平均回收率为74.5%~106.7%,检出限为0.2~204.2 ng/g。结论:此方法测定快速、准确、灵敏度高、分离度高,可用于减肥类保健食品中27种违法添加化学药品的检测。
Objective: To develop detection method for the simultaneous screening and confirmation of 27 illegally added in slimming health food using high performance liquid chromatography-tandem mass spectrometry( HPLC-MS/MS).Methods: The chemical drugs were separated on an Agilent Eclipse Plus C_(18) chromatographic column( 2.1 mm × 100 mm,1.8 μm) with acetonitrile and aqueous solution of 10 mmol/L ammonium acetate( adjust to p H4.0 with formic acid) as mobile phase under gradient elution at a flow rate of 0.2 m L/min.The 27 illegally added in slimming health food were conducted qualitatively and quantitatively analysis by tandem mass spectrometry under multiple reaction monitoring( MRM) mode.Results: The method was linear with correlation coefficients( R~2) which were not less than 0.99,and the precision expressed as relative standard deviations( RSDs) were not more than 8.0%.The recoveries of 27 drugs illegally added in slimming health food at different spiked concentrations ranged from 74.5% to 106.7%.The limits of detection( LODs) were in the range of 0.2 ~ 204.2 ng/g.Conclusion: This method is rapid,accurate and sensitive with a high degree of separation,and can be used for the detection of the 27 illegally added chemicals in slimming health foods.
Objective: To develop detection method for the simultaneous screening and confirmation of 27 illegally added in slimming health food using high performance liquid chromatography-tandem mass spectrometry( HPLC-MS/MS).Methods: The chemical drugs were separated on an Agilent Eclipse Plus C_(18) chromatographic column( 2.1 mm × 100 mm,1.8 μm) with acetonitrile and aqueous solution of 10 mmol/L ammonium acetate( adjust to p H4.0 with formic acid) as mobile phase under gradient elution at a flow rate of 0.2 m L/min.The 27 illegally added in slimming health food were conducted qualitatively and quantitatively analysis by tandem mass spectrometry under multiple reaction monitoring( MRM) mode.Results: The method was linear with correlation coefficients( R~2) which were not less than 0.99,and the precision expressed as relative standard deviations( RSDs) were not more than 8.0%.The recoveries of 27 drugs illegally added in slimming health food at different spiked concentrations ranged from 74.5% to 106.7%.The limits of detection( LODs) were in the range of 0.2 ~ 204.2 ng/g.Conclusion: This method is rapid,accurate and sensitive with a high degree of separation,and can be used for the detection of the 27 illegally added chemicals in slimming health foods.
引文
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[13]王柯,胡青,崔益冷,等.液相色谱-离子阱质谱联用检测减肥类中药及保健食品中28种非法掺家药物的研究[J].药物分析杂志,2008,28(8):1268-1274.
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[18]蔡亚玲,Clive Barwell,阮金兰.高效液相色谱法对氨苯蝶啶等7种利尿药的分离测定[J].医药导报,2004,23(6):413-414.
[19]陈海滨,吴春敏,胡敏,等.LC-MS/MS检测降压类中药制剂中非法添加的9种化学药物[J].海峡药学,2012,24(9):47-50.
[20]刘萍,王本杰,魏春敏,等.人血浆中螺内酯及其代谢物坎利酮的LC-MS测定[J].中国医药工业杂志,2008,39(11):842-845.
[2]鞠瑞秀,王慎田.减肥药的副作用及合理应用[J].实用医技杂志,2004,11(5):804-805.
[3]李萍,高向军,周娟.薄层色谱法测定止咳平喘胶囊中麻黄碱的含量[J].华西药学杂志,1999,14(2):60-61.
[4]Etil Ariburnu,Mehmet Fazli Uludag,Huseyin Yalcinkaya,et al.Comparative determination of sibutramine as an adulterant in natural slimming products by HPLC and HPTLC densitometry[J],Journal of Pharmaceutical and Biomedical Analysis,2012,64-65:77-81.
[5]于海霞,李露,马慧芬,等.毛细管电泳法测定螺内酯片剂中螺内酯的含量[J].山西医科大学学报,2015,46(10):995-998.
[6]葛宝坤,张群谦,赵孔祥.高效液相色谱法同时测定减肥类保健食品中盐酸西布曲明和酚酞[J].药物分析杂志,2012,32(11):2034-2037.
[7]薛丰,李阳,王媛.高效液相色谱法同时测定功能食品中6种违禁成分[J].四川大学学报(医学版),2013,44(1):135-138.
[8]王静文,黄湘鹭,曹进,等.超高效液相色谱法同时测定减肥类保健食品中非法添加的25种药物[J].色谱,2014,32(2):151-156.
[9]朱志鑫,吴惠勤,黄晓兰,等.气相色谱-质谱法检测减肥食品中芬氟拉明和西布曲明[J].现代食品科技,2012,28(10):1419-1422.
[10]陈稚,吴都督.HPLC/ESI-MS测定减肥保健食品中的双去甲基西布曲明[J].中国食品卫生杂志,2010,22(1):24-26.
[11]钮正睿,张庆生,曹进.超高效液相色谱-串联质谱法快速检测保健食品中非法添加的6种减肥类化学成分的研究[J].中国实验方剂学杂志,2014,20(18):91-94.
[12]马微,马强,付丽,等.高效液相色谱-串联质谱法同时测定减肥保健食品中非法添加的药物利莫那班和奥利司他[J].色谱,2010,28(1):43-48.
[13]王柯,胡青,崔益冷,等.液相色谱-离子阱质谱联用检测减肥类中药及保健食品中28种非法掺家药物的研究[J].药物分析杂志,2008,28(8):1268-1274.
[14]康银花,晋展.新型减肥药Lorcaserin Hydrochloride[J].药学进展,2008,32(9):423-425.
[15]马微,马丽卿,付丽,等.减肥类保健食品中添加违禁药物的研究现状[J].中国卫生检验杂志,2009,19(12):3023-3026.
[16]徐耿明,韦莉萍.减肥药的研究进展[J].第一军医大学分校学报,2004,27(2):212-214.
[17]Leandro M.de Carvalho,Mariele Martini,Ana Paula L.et al.Presence of synthetic pharmaceuticals as adulterants in slimming phytotherapeutic formulations and their analytical determination[J].Forensic Science International,2011,204:6-12.
[18]蔡亚玲,Clive Barwell,阮金兰.高效液相色谱法对氨苯蝶啶等7种利尿药的分离测定[J].医药导报,2004,23(6):413-414.
[19]陈海滨,吴春敏,胡敏,等.LC-MS/MS检测降压类中药制剂中非法添加的9种化学药物[J].海峡药学,2012,24(9):47-50.
[20]刘萍,王本杰,魏春敏,等.人血浆中螺内酯及其代谢物坎利酮的LC-MS测定[J].中国医药工业杂志,2008,39(11):842-845.