摘要
应用高效液相色谱-光电二极管阵列检测法(HPLC-PDA),建立了检测补肾壮阳类保健品和中成药中非法添加的14种化学药物的方法,涵盖补充检验方法中的11种5-型磷酸二酯酶抑制剂和典型的3种5-羟色胺再摄取抑制。样品经乙腈超声提取后,采用Agilent 5 HC-C18(2)色谱柱(250 mm×4.6 mm,5μm),以乙腈-甲醇-乙酸铵溶液(pH值分别为5.0和7.0)为流动相,进行梯度洗脱,流速1.0 mL/min,柱温30℃,进样量10μL,PDA检测器在190~400 nm范围内扫描,254、238 nm监测,外标法定量。检测的阳性样品以UPLC-MS/MS进行确证,ESI源,正离子模式,MRM扫描。结果表明,14种化学药物均能够完全分离,在考察的质量浓度范围内线性关系良好(r>0.9999),低、中、高3个目标物浓度的平均回收率(n=9)为99.9%~101.0%,相对标准偏差均小于2%,检测限为0.016~0.201μg/mL。91批样品中共检出阳性样品7批,非法添加药物3种。通过UPLC-MS/MS均能够得到确证。该方法操作简便、专属性强、结果准确、灵敏度高,适用于日常监管检验。
A high performance liquid chromatography-photodiode array detection(HPLC-PDA)method was established for detecting 14 chemical drugs illegally added to health products and Chinese patent medicines for sexual enhancement.The detected compounds comprised 11 phosphodiesterase inhibitors that met the supplementary test criteria,as well as three typical serotonin reuptake inhibitors.The samples were extracted with acetonitrile and then separated using an Agilent 5 HC-C18(2)chromatographic column(250 mm×4.6 mm,5μm)through gradient elution with a mobile phase consisting of acetonitrile,methanol,ammonium,and acetate.The mobile phase pH was 5.0 and 7.0,flow velocity was 1.0 mL/min,column temperature was 30℃,sample size was 10μL,PDA detector scanning range was 190~400 nm,monitoring was conducted at 254 and 238 nm,and the compounds were quantified using an external standard.The separation of 14 chemical drugs was adequate,the linear relationship was good within a certain concentration range,and the correlation coefficient r was>0.9999.The average recoveries(n=9)of low,medium,and high concentrations were 99.9%~101.0%with RSD<2%,and the detection limit was 0.016~0.201μg/mL.A total of seven positive samples were detected in 91 batches of marketed products;the addition of three compounds was illegal.The method is simple,accurate,specific,and sensitive;therefore,it is suitable for daily supervision and inspection.
作者
李榕
朱斌
耿昭
张文波
刘隆兴
LI Rong;ZHU Bin;GENG Zhao;ZHANG Wenbo;LIU Longxing(Bazhong Product Inspection and Testing Center,Bazhong 636000,China;Sichuan Institute for Drug Control(Sichuan Testing Center of Medical Devices),NMPA Key Laboratory for Quality Evaluation for Traditional Chinese Medicine,Chengdu 611731,China)
出处
《现代食品科技》
北大核心
2025年第1期320-330,共11页
Modern Food Science and Technology
基金
四川省药品监督管理局药品科技项目(2023005)。
