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目的:建立清血内消丸中马兜铃酸A的限量检查法。方法:采用1%碳酸钠溶液多次加热溶解样品,用三氯甲烷多次提取,弃去三氯甲烷层,碱水层用稀盐酸调pH,加三氯甲烷提取多次,收集合并三氯甲烷层,蒸干,残渣加甲醇溶解,精密吸取1 mL,置20 mL量瓶,加乙腈-水(40∶60)稀释至刻度,以水(0.1%甲酸+5 mmol.L-1甲酸铵)/(%)和乙腈(含5%水,0.1%甲酸+5 mmol.L-1甲酸铵)/(%)为流动相梯度洗脱,应用高效液相色谱/电喷雾质谱多离子反应监测模式(MRM)测定。结果:马兜铃酸A在11.21～299.0 pg进样量与马兜铃酸A峰面积呈良好的线性关系(r=0.999 5),检测限0.1μg.L-1,定测限0.3μg.L-1,平均回收率119.20%,RSD 4.0%(n=9)。结论:方法准确,快速,简便,重复性好,干扰少,特异性好,能满足马兜铃酸A的痕量残留的检测要求。
Objective: To establish a limit test method for aristolochic acid A in Qingxue Neoxiao pill. Methods: The sample was dissolved by repeated heating with 1% sodium carbonate solution and extracted repeatedly with chloroform. The chloroform layer was discarded. The aqueous layer was adjusted to pH with dilute hydrochloric acid and extracted with chloroform three times. The methane layer was evaporated to dryness and the residue was dissolved in methanol. The precision of the extraction was 1 mL and the 20 mL volumetric flask was diluted with acetonitrile-water (40:60) to the mark. Water (0.1% formic acid + 5 mmol.L-1 ammonium formate ) And acetonitrile (containing 5% water, 0.1% formic acid and 5 mmol·L-1 ammonium formate) / (%) as mobile phases. The mobile phases were eluted with high performance liquid chromatography / electrospray ionization mass spectrometry Mode (MRM) assay. RESULTS: The linear range of aristolochic acid A injection ranged from 11.21 ~ 299.0 pg to peak area of aristolochic acid A (r = 0.999 5). The limit of detection was 0.1 μg.L-1. The limit of quantification was 0.3 μg. L-1, the average recovery was 119.20%, RSD 4.0% (n = 9). Conclusion: The method is accurate, rapid, simple, reproducible, less perturbed and has good specificity and can meet the detection requirements of trace residues of aristolochic acid.