固相萃取-多波长超高效液相色谱法同时测定咳喘宁中5种生物碱类成分的含量

Simultaneous determination of 5 kinds of alkaloids in Kechuanning tablets by SPE-UPLC under different UV-vis wavelength

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。

The paper is to establish a method for simultaneous determination of 5 kinds of alkaloids in ephedra and poppy which are in Kechuanning tablets. Solid-phase extraction （SPE） was adopted in pretreatment, and a UPLC method with 2 different wavelengths had been developed： 210 nm for the detection of morphine, codeine phosphate, ephedrine hydrochloride and pseudoephedrine hydrochloride, and 251 nm for papaverine hydrochloride. The column used was Acquity UPLC BEH C18 （100 mm x 2.1 mm ID, 1.7μm） with linear gradient elution using acetonitrile and 0.1% phosphoric acid. The flow rate was 0.4 mL.min-1, and the column temperature was 30 ~C. The linear response range was 0.375 0 - 12.50 μg·mL^-l for morphine, 0.064 32 - 2.144 μg·mL^-1 for codeine phosphate, 0.030 06 - 1.002 μg·mL^-1 for papaverine hydrochloride, 1.126 - 37.52 μg·mL^-1 for ephedrine hydrochloride, 0.287 8 - 9.592 μg·mL^-1 for pseudoephedrine hydrochloride （r = 0.999 7）. The average recoveries of these compounds were 99.26%, 100.6%, 95.29%, 100.1% and 97.48%, respectively. This is a more reasonable and credible method of quality control for Kechuanning tablets.