摘要
目的建立补肾抗疲劳类中成药及保健食品中非法添加9种5型磷酸二酯酶(PDE-5)抑制剂及其衍生物的超高效液相色谱-串联三重四级杆质谱(UPLC-MS/MS)快速检测方法。方法采用Agilent Zorbax SB C18(100 mm×2.1 mm,1.8μm)色谱柱分离,以乙腈-10 mmol·L^(-1)乙酸铵(含体积分数0.1%甲酸)为流动相,梯度洗脱,在电喷雾离子化正离子模式下,以动态多反应监测模式(DMRM)检测。结果 9种PDE-5抑制剂及其衍生物在相应浓度范围内与峰面积均呈良好线性关系,r均大于0.998,检测限(S/N=3)为0.03~0.22 ng·mL^(-1),3个浓度水平回收率均在92.4%~109.8%,RSD均在0.70%~4.0%(n=6)。收集的86批样品中有58批呈非法添加阳性。结论本方法快速,准确,灵敏度高和专属性强,可用于补肾抗疲劳类中成药及保健食品中9种PDE-5抑制剂及其衍生物的定性筛查和定量检测。
Objective To develop a method for the simultaneous determination of 9 phosphodiesterase-5 inhibitors which were illegally added to invigorant herbal medicines and dietary supplements by UPLC-MS/ MS. Methods Samples was separated on an Agilent Zorbax SB C18 （100 mm×2.1 mm, 1.8 μm） column with gradient elution. The mobile phase consisted of acetonitrile-10 mmol · L- 1 ammonium acetate water solution containing 0.1% formic acid. Electrospray ionization source in positive ion mode was used to analyze 9 phosphodiesterase-5 inhibitors in the dynamic multiple reaction monitoring mode. Results A good resolution of 9 phosphodiesterase-5 inhibitors was obtained. The correlation coefficients within the linearity were above 0.998. The limits of detection （S/N=3） ranged 0.03 -- 0.22 ng·mL- 1. The average recoveries were at 92.4%-109.8% with relative standard deviations at 0.70%-4.0% （n = 6） at 3 spiked levels. Illegal addition of chemical drugs was found in 58 of the 86 tested samples. Conclusion The method is rapid, accurate, sensitive and suitable for the confirmation of 9 illegally added phosphodiesterase-5 inhibitors in invigorant herbal medicines and dietary supplements.
作者
倪赞
张崇生
NI Zan;ZHANG Chong-sheng(Wenzhou Institute for Food and Drug Control,Wenzhou Zhejiang 32500)
出处
《中南药学》
CAS
2018年第9期1295-1299,共5页
Central South Pharmacy
作者简介
倪赞，男，主管药师，主要从事药物分析方面研究，Tel：（0577）88509531，E-mail：ni_zan@163．com;通讯作者：张崇生，男，副主任药师，主要从事药物分析方面研究，Tel：（0577）88536561，E-mail：1018763742@qq．com
