中成药和保健食品中9种5型磷酸二酯酶.PDFVIP

国际中医中药杂志2016年12月第38卷第12期 Int J Trad Chin Med, December 2016, Vol. 38, No. 12 ·1107 · ·论著· 中成药和保健食品中9 种5 型磷酸二酯酶 抑制剂的液相色谱-高分辨质谱检测法 郭晓芳 马黄璜 武金荣 【摘要】 目的 采用分散固相萃取技术结合超高效液相色谱-高分辨质谱法建立中成药和保健食品 中9 种5 型磷酸二酯酶(phosphodiesteras 5, PDE5)抑制剂的检测方法。方法 用0.1% 甲酸-乙腈超声提取 后，经磁性复合填料分散固相萃取法净化，以C18 色谱柱进行色谱分离，通过高分辨质谱的全扫描/实时 二级质谱扫描进行分析检测。结果 9 种 PDE5 抑制剂在 5～500 ng/L 范围内呈良好的线性关系(r ＞ 0.999)。9 种PDE5 抑制剂的方法检出限和最低定量限分别为2 、5 μg/kg 。空白样品在5～500 μg/kg 范围 内的3 个加标水平的平均回收率为87.6%～108.9%，相对标准偏差为1.9%～7.2% 。应用该方法对中成药 和保健食品实际样品进行检测，有 1 份样品检出豪莫西地那非非法添加。结论 本方法适用于中成药和 保健食品中9 种PDE5 抑制剂的快速筛查和定量检测。 【关键词】 中成药；保健食品；固相萃取；高分辨质谱；5 型磷酸二酯酶抑制剂 Determination of 9 PDE5 inhibitors in Chinese patent medicines and dietary supplements by UHPLC-HRMS Guo Xiaofang, Ma Huanghuang, Wu Jinrong. Department of Pharmacy, Peoples Hospital Affiliated to Fujian University of Traditional Chinese Medicine, Fuzhou 350004, China Corresponding author: Guo Xiaofang, Email: 2686669747@ 【Abstract 】 Objective The method for simultaneous determination of 9 PDE5 inhibitors in Chinese patent medicines and dietary supplements was developed using the UPLC-HRMS coupled with d-SPE technique. Methods The samples were extracted with 0.1% acidic acetonitrile and cleaned up with d-SPE by using mixture of C , PSA and magnetic Fe O as sorbents. The analyses were operated under Full Scan/ddms2 18 3 4 by HRMS. Results The results showed a good linearity in the range of 5-500 ng/L (r0.999). The LODs and LOQs for the 9 PDE5 inhibitors were 2 μg/kg and 5 μg/kg, respectively. The recovery results at the levels of 5-500 μg/kg were satisfied with average recovery rates of 87.6%-108.9% and the RSD of 1.9%-7.2%. The method was applied for the determination of