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作 者:勾新磊[1] 高峡[1,2] 胡光辉[1] 刘伟丽[1,2]
机构地区:[1]北京市理化分析测试中心,北京100089 [2]国家食品质量安全监督检验中心,北京100094
出 处:《色谱》2014年第8期822-826,共5页Chinese Journal of Chromatography
基 金:北京市自然科学基金项目(2122018);北京市科学技术研究院创新团队计划项目(IG200801N/C2)
摘 要:建立了同时测定中成药和保健品中9种抗抑郁药物的超高效液相色谱-串联质谱( UPLC-MS / MS)分析方法。以甲醇为提取溶剂,超声提取,离心后取上清液,使用 Waters ACQUITY UPLC BEH C 18色谱柱(100 mm×2.1 mm,1.7μm)进行分离,以乙腈和0.1%(v / v)甲酸水为流动相对目标物进行梯度洗脱。在电喷雾正离子模式下,采用多反应监测(MRM)模式进行定性和定量分析。结果表明,9种抗抑郁药物在0.04~20μg / L 范围内线性关系良好,线性相关系数(R2)均大于0.998;目标物的检出限为0.0068~0.034μg / L;在0.5、1、5μg / L 3个添加水平下的平均回收率为77.7%~100.8%,相对标准偏差为0.9%~9.1%。本方法准确、简便、快速,可用于中成药和保健品中抗抑郁药物的检测。A sensitive method was developed for the simultaneous determination of nine antide-pressants in traditional Chinese medicines and health food by ultra performance liquid chroma-tography-tandem mass spectrometry( UPLC-MS / MS)based on the sonication-assisted extrac-tion. The separation was performed on a Waters ACQUITY UPLC BEH C 18 column(100 mm×2. 1 mm,1. 7 μm)by using 0. 1%(v / v)formic acid aqueous solution and acetonitrile as the mobile phases with gradient elution at a flow rate of 0. 2 mL / min. The electrospray ionization( ESI) source in positive ion mode was used for the analysis of the nine antidepressants in the multiple reaction monitoring( MRM ) mode. The standard curves for the nine antidepressants were obtained with good correlation coefficients( R 2 ﹥0. 998)in the concentration range of 0. 04-20μg / L. The limits of detection for the nine antidepressants were in the range of 0. 006 8- 0. 034μg / L. The average recoveries at three spiked levels( 0. 5,1,5 μg / L)were 77. 7% - 100. 8%with the relative standard deviation of 0. 9% -9. 1% . The method is accurate,simple,rapid and feasible for the simultaneous determination of the antidepressants in traditional Chinese medi-cines and health food.
关 键 词:超高效液相色谱-串联质谱 抗抑郁药物 中成药 保健品
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