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建立咳喘宁中罂粟壳和麻黄所含5种主要生物碱类成分的含量测定方法。样品经固相萃取后用超高效液相色谱法测定,色谱柱为Acquity UPLC BEH C18(100 mm×2.1 mm ID,1.7μm),流动相为乙腈与0.1%磷酸溶液梯度洗脱,检测波长为210 nm(吗啡、磷酸可待因、盐酸麻黄碱和盐酸伪麻黄碱)与251 nm(盐酸罂粟碱),流速0.4 mL·min-1,柱温30℃。结果显示,吗啡、磷酸可待因、盐酸罂粟碱、盐酸麻黄碱和盐酸伪麻黄碱分别在0.375 0～12.50、0.064 32～2.144、0.030 06～1.002、1.126～37.52、0.287 8～9.592μg·mL-1内具有良好的线性关系(r=0.999 7),平均回收率分别为(n=9)99.26%、100.6%、95.29%、100.1%和97.48%。该方法快速、准确、重复性好,可为咳喘宁的质量控制提供快速准确的检测。
To establish the method for the determination of five main alkaloids contained in Kechuanning in poppy and ephedra. The sample was subjected to SPE and determined by ultra performance liquid chromatography. The column was Acquity UPLC BEH C18 (100 mm × 2.1 mm ID, 1.7 μm). The mobile phase consisted of a gradient elution of acetonitrile and 0.1% phosphoric acid. The detection wavelength was 210 nm (morphine, codeine phosphate, ephedrine hydrochloride and pseudoephedrine hydrochloride) and 251 nm (papaverine hydrochloride) at a flow rate of 0.4 mL · min-1 at a column temperature of 30 ° C. The results showed that morphine, codeine phosphate, papaverine hydrochloride, ephedrine hydrochloride and pseudoephedrine hydrochloride were in the range of 0.375 0 ~ 12.50,0.064 32 ~ 2.144,0.030 06 ~ 1.002,1.126 ~ 37.52,0.287 8 ~ 9.592μg · mL -1 (R = 0.999 7). The average recoveries were 99.26%, 100.6%, 95.29%, 100.1% and 97.48%, respectively. The method is rapid, accurate and reproducible and can provide fast and accurate detection of Kechuanning’s quality control.