Liu Yong-li, Li Dong-mei, Feng Li, Yuan Hao
Hebei Provincial Institute for Drug Control, Shijiazhuang 050011, China.
Yao Xue Xue Bao. 2011 May;46(5):581-5.
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, 1.7 microm) 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 degrees C. The linear response range was 0.375 0 - 12.50 microg.mL-1 for morphine, 0.064 32 - 2.144 microg.mL-1 for codeine phosphate, 0.030 06 - 1.002 microg.mL-1 for papaverine hydrochloride, 1.126 - 37.52 microg.mL-1 for ephedrine hydrochloride, 0.287 8 - 9.592 microg.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.
本文旨在建立一种同时测定克喘宁片中麻黄和罂粟中5种生物碱的方法。预处理采用固相萃取(SPE),并开发了一种具有2种不同波长的超高效液相色谱(UPLC)方法:210 nm用于检测吗啡、磷酸可待因、盐酸麻黄碱和盐酸伪麻黄碱,251 nm用于检测盐酸罂粟碱。所用色谱柱为Acquity UPLC BEH C18(100 mm×2.1 mm内径,1.7μm),采用乙腈和0.1%磷酸进行线性梯度洗脱。流速为0.4 mL·min-1,柱温为30℃。吗啡的线性响应范围为0.375 0 - 12.50μg·mL-1,磷酸可待因的线性响应范围为0.064 32 - 2.144μg·mL-1,盐酸罂粟碱的线性响应范围为0.030 06 - 1.002μg·mL-1,盐酸麻黄碱的线性响应范围为1.126 - 37.52μg·mL-1,盐酸伪麻黄碱的线性响应范围为0.287 8 - 9.592μg·mL-1(r = 0.999 7)。这些化合物的平均回收率分别为99.26%、100.6%、95.29%、100.1%和97.48%。这是一种更合理、可靠的克喘宁片质量控制方法。