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目的:建立麻黄止嗽丸马兜铃酸A的限量检测方法。方法:样品经过固相萃取小柱进行处理,采用HPLC法,以Phenomenex Luna C18柱(4.6 mm×250 mm,5μm)为色谱柱,以乙腈:0.2%碳酸铵溶液(稀盐酸调节p H值=7.5)为流动相,采用梯度洗脱,流速:1.0 m L·min-1,柱温:35℃,检测波长:250 nm。结果:马兜铃酸A在0.006~0.120μg/m L浓度范围内有良好线性关系(r=0.9999),检测限(S/N=3)为1.0 ng/m L,定量限(S/N=10)为3.0 ng/m L平均加样回收率为96.4%。结论:本方法灵敏度高、准确、重复性好、专属性强,可用于麻黄止嗽丸限量测定马兜铃酸A的限量。
Objective: To establish a method for the determination of aristolochic acid A in Mahuang Cough Pill. Methods: The samples were subjected to solid-phase extraction (SPE) cartridges. HPLC was performed on a Phenomenex Luna C18 column (4.6 mm × 250 mm, 5 μm) with acetonitrile: 0.2% ammonium carbonate solution 7.5) as mobile phase. The gradient elution was carried out at a flow rate of 1.0 mL · min -1. The column temperature was 35 ℃ and the detection wavelength was 250 nm. RESULTS: The calibration curve of aristolochic acid A showed good linearity (r = 0.9999) in the concentration range of 0.006-0.120μg / m L with the detection limit (S / N = 3) of 1.0 ng / = 10) was 3.0 ng / m L The average recovery was 96.4%. Conclusion: The method has high sensitivity, accuracy, repeatability and specificity. It can be used for the limited determination of aristolochic acid A in Mahuang Zhiluowan.