中药及保健食品中新型PDE_5抑制剂的检测研究  

Study on the detection of new PDE_5 inhibitor in traditional Chinese medicine and health food

作　　者：吴燕[1] 李华龙[1] 米亚娴[1] 邵建强[1] 

机构地区：[1]天津市药品检验所,天津300070

出　　处：《药物分析杂志》2016年第1期117-121,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:优化和建立中药及保健食品中非法添加新的5型磷酸二酯酶(PDE_5)抑制剂—丙氧苯基硫代羟基豪莫西地那非的检测方法。方法:分别建立HPLC-MS/MS联用法和HPLC法进行丙氧苯基硫代羟基豪莫西地那非的定性及定量分析。HPLC-MS/MS联用法:采用Waters XBridge^(TM)ODS(2.1 mm×100 mm,3.5μm)色谱柱,以含15%乙腈、0.1%乙酸的0.02 mol·L^(-1),乙酸铵(A)-含15%乙腈的甲醇(B)为流动相,梯度洗脱(0~15 min,12%B→30%B;15~25 min,30%B→65%B;25~35 min,65%B;35~40 min,65%B→12%B),流速0.2 mL·min^(-1),正离子模式,氮气为雾化气,雾化气流量3 L·min^(-1),空气为加热气,加热气流量10 L·min^(-1),接口温度300℃,DL温度250℃,加热模块温度400℃。HPLC法:采用资生堂CAPCELL PAK C_(18)MGII(4.6 mm×150 mm,5μm)色谱柱,以0.1%三氟乙酸水溶液(A)-0.1%三氟乙酸乙腈溶液(B)为流动相,梯度洗脱(0~15 min,10%B→90%B;15~20 min,90%B;20~20.1 min,90%B→10%B),流速1.0 mL·min^(-1),检测波长230 nm。结果:HPLC-MS/MS联用法用于丙氧苯基硫代羟基豪莫西地那非的定性检测,考察了质谱确证参数;HPLC法用于丙氧苯基硫代羟基豪莫西地那非的定量分析,考察了该物质相对于西地那非的校正因子,提高方法适用性。结论:该法用于中药及保健食品中新型PDE_5抑制剂的检测,专属性强,具有实践意义。Objective:To develop a method for detecting new phosphodiesterase type 5 inhibitors(PDE_5)inhibitor(propoxyphenyl-thiohydroxyhomosil) that illegally added in traditional Chinese medicine and health food.Methods:HPLC-MS/MS and HPLC were adopted as qualitative and quantitative methods for propoxyphenyl-thiohydroxyhomosil separately.HPLC-MS/MS method was carried out on a Waters XBridge^(TM)ODS column(2.1 mm×100 mm,3.5 μm) with mobile phase at a flow rate of 0.2 mL· min^(-1).The mobile phase consisted of 0.02 mol· L^(-1) ammonium acetate including 15%acetonitrile and 0.1%acetic acid(A)-methanol including 15%acetonitrile(B),and the ratios of B were 12%→30%at 0-15 min,30%→65%at 15-25 min,65%at 25-35 min,65%-12%at 35-40 min.A positive electrospray ion mode was used with nitrogen as the desolvation gas and air as the dry gas,nebulizing gas flow was 3 L· min^(-1),heating gas flow was 10 L· min^(-1),interface temperature was 300 ℃,DL temperature was 250 ℃,and the heat block temperature was 400 ℃;HPLC method was performed on a CAPCELL PAK C_(18)MGⅡ column(150 mm×4.6 mm,5 μm) with mobile phase at a flow rate of 1.0 mL· min^(-1),and the detection wavelength was 230 nm.The mobile phase was 0.1%trifluoroacetic acid(A)-acetonitrile including 0.1%trifluoroacetic acid(B) and the ratios of B were 10%→90%at 0-15 min,90%at 15-20 min and 90%-10%at 20-20.1 min.Results:The HPLC-MS/MS method was optimized for qualitative detection of propoxyphenyl-thiohydroxyhomosil.The quantitative method(HPLC) was developed.The calibration factor of propoxyphenyl-thiohydroxyhomosil to sildenafil was determined to improve the convenience of the method.Conclusion:The established method is high efficient,specific,which can be used for detection of new PDE_5 inhibitor that illegally added in traditional Chinese medicine and health food.

关 键 词：中药 保健食品 5型磷酸二酯酶抑制剂(PDE 抑制剂) 非法添加 丙氧苯基硫代羟基豪莫西地那非 液相色谱-质谱-质谱联用 高效液相色谱 

分 类 号：R917[医药卫生—药物分析学]