中国广州分析测试中心广东省分析测试技术公共实验室
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黄芳, 吴惠勤, 黄晓兰, 等. 高效液相色谱-串联质谱法同时测定保健品中非法添加的六种减肥化学品[J]. 分析测试学报, 2013,32(6):699-704.
Simultaneous Determination of Six Chemical Drugs Illegally Added in Dietary Supplement by High Performance Liquid Chromatography Tandem Mass Spectrometry[J]. 2013,32(6):699-704.
建立了保健品中奥利司他、利莫那班、N-去二甲基西布曲明、酚酞、西布曲明、芬氟拉明6种常见减肥化学品的高效液相色谱-串联质谱测定方法。实验优化了前处理方法、液相色谱条件和质谱参数。样品经甲醇提取后,采用C8色谱柱分离,乙腈-水(含有10 mmol/L乙酸铵)为流动相梯度洗脱,流速0.3 mL/min。采用正离子模式的电喷雾质谱检测,多反应选择离子监测(MRM)。方法的检出限达到0.5 μg/L,6种化合物在0.001 ~0.5 mg/L范围内线性关系良好,相关系数均大于0.999。低、中、高3个加标水平的平均回收率为81%~100%,相对标准偏差为4.8%~6.9%。方法简便、快速、准确可靠,已应用于保健品中非法添加减肥药的检测及筛查。
A high performance liquid chromatography-mass spectrometric(HPLC-MS/MS) method was proposed for the determination of 6 anti-obesity chemical drugs(sibutramine,N-di-desmethyl sibutramine,fenfluramine,phenolphthalein,rimonabant,orlistat)added illegally into health foods.The conditions of extraction procedures and the parameters of HPLC-MS/MS were optimized.The drugs were extracted with methanol,and separated on a C8 chromatographic column using a mixture of acetonitrile and 10 mmol/L ammonium acetate solution as mobile phase with gradient elution.The detection of 6 targeted compounds was performed by positive-ion electrospray ionization mass spectrometry(ESI MS) under multiple reaction monitoring(MRM) mode.Good linearities for 6 compounds were obtained in the range of 0.001-0.5 mg/L with correlation coefficients greater than 0.999.The spiked recoveries were in the range of 81%- 100%with RSDs of 4.8%-6.9%.The detection limits of these drugs were up to 0.5 μg?L-1.The results indicated that this method was simple,rapid and accurate,and was successfully applied in the examination of examine chemical drugs illegally added in the dietary supplement.
减肥药液相色谱-串联质谱保健品
weight-loss chemical drugshigh performance liquid chromatography-tandem mass spectrum(HPLC-MS/MS)functional foods
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