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目的建立超高效液相色谱法同时测定肉蔻四神丸中吗啡、可待因与罂粟碱含量的方法。方法样品提取后经固相萃取柱去除杂质干扰。色谱条件:色谱柱为Waters Acquity C18 BEH(2.1 mm×100 mm,1.7μm),以乙腈与0.1%磷酸溶液梯度洗脱为流动相,检测波长为210 nm(吗啡、磷酸可待因)与251 nm(盐酸罂粟碱),流速0.4 mL.min-1,柱温30℃。结果吗啡、磷酸可待因、盐酸罂粟碱分别在0.514 0～10.28、0.254 5～5.090、0.050 5～1.010μg.mL-1内呈良好的线性关系,相关系数r为0.999 9,回收率分别为99.51%、98.18%、100.7%。结论该方法准确、灵敏、重现性好,可用于肉蔻四神丸的质量控制。
OBJECTIVE To establish a method for the simultaneous determination of morphine, codeine and papaverine in meatball Sishen pill by ultra performance liquid chromatography. Methods Samples were extracted by solid phase extraction column to remove impurities. Chromatographic conditions: The column was Waters Acquity C18 BEH (2.1 mm × 100 mm, 1.7 μm). The mobile phase was eluted with a gradient of acetonitrile and 0.1% phosphoric acid. The detection wavelength was 210 nm (morphine phosphate codeine) nm (papaverine hydrochloride), the flow rate of 0.4 mL.min-1, column temperature 30 ℃. Results There was a good linear relationship between morphine, codeine phosphate and papaverine hydrochloride in the ranges of 0.514 0-10.28,0.254 5-5.090,0.050 5-1.010 μg.mL-1 with the correlation coefficient r of 0.999 9. The recoveries were 99.51%, 98.18%, 100.7%. Conclusion The method is accurate, sensitive and reproducible. It can be used for the quality control of Meikoshishen pill.