聚合物整体柱固相微萃取-高效液相色谱法测定中成药和保健食品中枸橼酸西地那非

Determination of Sildenafil Adulterants in Traditional Chinese Medicines and Health Foods by Polymer Monolith Microextraction Coupled with High Performance Liquid Chromatography

采用聚(甲基丙烯酸-乙二醇二甲基丙烯酸酯)聚合物整体柱固相微萃取(PMME),并与高效液相色谱联用,建立了中成药中枸橼酸西地那非的检测方法。实验优化了影响萃取效率的因素,包括萃取流速、萃取体积、样品基质pH值等参数。中成药样品经溶解和过滤后可直接进行分离分析。结果表明,枸橼酸西地那非在0.5～50μg/mL的浓度范围内具有良好的线性关系,检出限为0.05μg/mL,日内、日间测定的相对标准偏差不高于9.7%。方法已成功地应用到实际样品检测中,其加标回收率大于83.40%。该方法简单、快速、灵敏度高,适用于中成药及保健品中西地那非的分析检测。

Adulteration of allegedly natural herbal medicines with undeclared synthetic drugs is a common and dangerous phenomenon of alternative medicine.The purpose of the study was to develop a novel method of polymer monolith microextraction（PMME） technique combined with high performance liquid chromatography for the rapid and sensitive determination of adulterant sildenafil in traditional Chinese medicines（TCMs）.To obtain the optimum extraction efficiency,several parameters related to PMME,including extraction flow rate,extraction volume,and pH value of the sample matrix were investigated.By simple dilution and filtering,the sample solution could be directly injected into the device for extraction.In this method,good linearities were obtained for sildenafil with the correlation coefficients（R2） above 0.99.The limit of detection of sildenafil in the herbal medicines was calculated to be 0.05 μg/mL.The recoveries of sildenafil in herbal medicine matrix ranged from 83.40% to 94.90%.Reproducibility of the method was exhibited by intra-and inter-day precisions,yielding the relative standard deviations less than 9.7%.The results demonstrated that the proposed method is simple,sensitive for the determination of sildenafil in TCMs and health foods.