Guo Xiaofang,Ma Huanghuang,Wu Jinrong..Determination of 9 PDE5 inhibitors in Chinese patent medicines and dietary supplements by UHPLC-HRMS[J].,2016,38(12):1107-1111.[doi:10.3760/cma.j.issn.1673-4246.2016.12.014]
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
- Title:
- Determination of 9 PDE5 inhibitors in Chinese patent medicines and dietary supplements by UHPLC-HRMS
- 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
- Keywords:
- Chinese patent drugs; Health food; Solid phase extraction; High resolution mass spectrometry; Phosphodiesteras 5 inhibitors
- 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。
- 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 C18, PSA and magnetic Fe3O4 as sorbents. The analyses were operated under Full Scan/ddms2 by HRMS. Results The results showed a good linearity in the range of 5-500 ng/L (r>0.999). 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 RSDs of 1.9%-7.2%. The method was applied for the determination of the real samples, and homosildenafil was detected as illegal addtives from the samples. Conclusion The results showed that the method was suitable for the analyses for 9 PDE5 inhibitors in Chinese patent medicines and dietary supplements.
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更新日期/Last Update:
2016-12-08