基于UPLC-MS/MS快速定量检测壮阳类中成药和保健品中非法添加物的研究

Based on UPLC-MS/MS Rapid Quantitative Detection Illegal Addition in Chinese Patent Medicines and Health Products

目的:建立以UPLC-MS/MS法检测壮阳类中成药和保健品中11种非法添加化学成分的方法,用于壮阳类中成药和保健品非法添加药品的检测。方法:以Waters Acquity BEH-C18柱(100mm×2.1mm,1.7μm)为色谱柱,乙腈-0.1%甲酸水溶液为流动相,2.5KV毛细管电压、200℃的脱溶剂温度和650L/hr的脱溶剂气流量为质谱条件下,0.3m L/min流速进行梯度洗脱。结果:11种化学成分的分离度较好;方法学考察中线性关系r均在0.995以上,加样回收率在90%~110%,最低检测限在0.20~3.86ng/m L范围内,定量限为0.57ng/m L^4.92ng/m L;在所检测的10种样品中,8种样品检测出含有西地那非。结论:UPLC-MS/MS法用于检测壮阳类中成药和保健品中非法添加11种化学成分快速、简便且效率高。

Objective:Establish a UPLC-ms/MS method to detect an aphrodisiac class 11 of proprietary Chinese medicines and health products is illegally added chemicals method,is used for an aphrodisiac kind of proprietary Chinese patent medicines and health products illegally added drug inspection.M ethod:A water Acquity BEH-C18 column(100 mm×2.1 mm,1.7 m)was used as chromatographic column,acetonitrile-0.1%acid aqueous solution as mobile phase,2.5 KVcapillary voltage,200℃desolvent temperature and 650 L/HR desolvent gas flow rate as mass spectrometry,and the flow rate of 0.3 m L/min was gradient eluted.Results:The separation of 11 chemical components is good;In methodology study,the linear relationship is above 0.995,review of standard sample recover90%-110%and the limit of determination(LOD)is in the range of 0.20 ng/ml^3.86 ng/ml and limit of quantitation(LOQ)is 0.57 ng/ml4.92 ng/ml.Sildenafil was detected in 8 of the 10 samples tested.Conclusion:UPLC-MS/MS method is rapid,simple and efficient for the detection of 11 illegal chemical ingredients in impotence Chinese patent medicines and health products.