色谱

色谱

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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

马微1,2*, 马强3, 付丽4, 马丽卿4, 王海波1, 柳彩云3, 唐英章3   

  1. 1.东宁出入境检验检疫局, 黑龙江 东宁157200; 2.中国农业大学, 北京100083; 3.中国检验检疫科学研究院, 北京100123; 4.郑州牧业工程高等学校, 河南 郑州 450011
  • 收稿日期:2009-05-10 修回日期:2009-07-10 出版日期:2010-01-28 发布日期:1981-09-25
  • 通讯作者: 马微
  • 基金资助:
    国家科技支撑计划农业领域课题项目No. 2006BAD27B02

Simultaneous determination of rimonabant and orlistat illegally added in the weight-loss functional foods by high performance liquid chromatography-tandem mass spectrometry

MA Wei1,2*, MA Qiang3, FU Li4, MA Liqing4, WANG Haibo1, LIU Caiyun3, TANG Yingzhang3   

  1. 1.Dongning Entry-Exist Inspection and Quarantine Bureau, Dongning 157200, China; 2.China Agriculture University, Beijing 100083, China; 3.Chinese Academy of Inspection and Quarantine, Beijing 100123, China; 4.Zhengzhou College of Animal Husbandry Engineering, Zhengzhou 450011, China
  • Received:2009-05-10 Revised:2009-07-10 Online:2010-01-28 Published:1981-09-25
  • Contact: MA Wei

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717

被引次数

29

摘要： 建立了一种专属、灵敏的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的高效液相色谱-串联质谱分析方法。不同类型的减肥保健食品经加速溶剂萃取后,用甲醇和10 mmol/L乙酸铵水溶液作流动相,采用梯度洗脱方式以Waters Atlantis T3色谱柱(150 mm×2.1 mm, 3 μm)分离,以电喷雾离子源正离子检测方式进行质谱分析。实验结果表明,利莫那班和奥利司他的方法检出限为0.5 mg/kg;在0.5～100 μg/L范围内呈良好的线性关系,相关系数分别为0.9989和0.9994;在2, 5, 10 mg/kg 3个添加水平范围内的平均回收率为80.5%～102.1%;日内精密度均小于6%,日间精密度均小于8%。同时研究了这两种药物的质谱特征,推测了其质谱裂解途径。本方法灵敏度高,重现性好,可用于不同类型减肥保健食品中非法添加的奥利司他和利莫那班的检测。

关键词: 奥利司他, 高效液相色谱-串联质谱法, 加速溶剂萃取, 减肥保健食品 , 利莫那班

Abstract: A sensitive and selective analytical method based on high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) has been developed for the simultaneous determination of rimonabant and orlistat in weight-loss functional foods. After the foods were extracted under accelerated solvent extraction, the HPLC separation was performed on a Waters Atlantis T3 column (150 mm × 2.1 mm, 3 μm) with a linear gradient elution program of methanol and 10 mmol/L ammonium acetate as the mobile phase. Electrospray ionization was applied and operated in the positive ion mode. The results showed that the limits of detection for the rimonabant and orlistat were 0.5 mg/kg. The calibration curves showed good linearities for rimonabant and orlistat in the range of 0.5~100 μg/L, and the correlative coefficients were 0.9989 and 0.9994, respectively. The mean recoveries at the 3 spiked levels (2, 5, 10 mg/kg) were 80.5%~102.1% with the intra-day precision less than 6% and the inter-day precision less than 8%. The work studied the mass spectrum characterization of the 2 drugs and speculated on the fragmentation pathways. The method is sensitive, reproducible and adapts to the determination of rimonabant and orlistat in different weight-loss functional foods.

Key words: accelerated solvent extraction, orlistat, rimonabant, weight-loss functional foods , high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)