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目的:建立消肿止痛酊中马兜铃酸A的限量检查法。方法:通过萃取、过固相萃取小柱对制剂中马兜铃酸A进行提取纯化,应用高效液相色谱法对其进行检测。色谱条件:采用HyperClone ODS 120A C18(4.6 mm×250 mm,5μm)色谱柱,流动相为0.3%碳酸铵溶液(用20%盐酸溶液调pH至7.5)-乙腈(80∶20),流速1.0 mL.min-1,检测波长250 nm。结果:马兜铃酸A进样量在0.2076～20.76 ng范围内线性关系良好(r=1.000);检测限(S/N=3)为0.21 ng.mL-1,定量限(S/N=10)为0.52 ng.mL-1;平均回收率(n=9)为90.1%。结论:所建立的方法简便快捷,重复性符合要求,结果准确可靠,可作为控制消肿止痛酊安全性的检测方法。
Objective: To establish a limited test method of aristolochic acid A in relieving pain and relieving pain. Methods: Aristolochic acid A was extracted and purified by supercritical phase extraction (SPE) cartridge, and its content was determined by high performance liquid chromatography (HPLC). Chromatographic conditions: The mobile phase consisted of 0.3% ammonium carbonate solution (adjusted to pH 7.5 with 20% hydrochloric acid) -acetonitrile (80:20) using a mobile phase of HyperClone ODS 120A C18 (4.6 mm × 250 mm, .min-1, detection wavelength 250 nm. RESULTS: The linear range was 0.2072 ~ 20.76 ng (r = 1.000). The limit of detection (S / N = 3) was 0.21 ng.mL- 10) was 0.52 ng.mL-1; the average recovery (n = 9) was 90.1%. Conclusion: The established method is simple, rapid and reproducible, and the results are accurate and reliable. It can be used as a test method to control the safety of detumescent analgesic tincture.