药学学报, 2011, 46(5): 581-585
引用本文:
刘永利 李冬梅 冯 丽 袁 浩. 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[J]. 药学学报, 2011, 46(5): 581-585.
LIU Yong-Li, Li-Dong-Mei, Feng- Li, Yuan- Gao. Simultaneous determination of 5 kinds of alkaloids in Kechuanning tablets by SPE-UPLC under different UV-vis wavelength[J]. Acta Pharmaceutica Sinica, 2011, 46(5): 581-585.

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
刘永利, 李冬梅, 冯 丽*, 袁 浩
(河北省药品检验所, 河北 石家庄 050011)
摘要:

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, 1.7 μm), 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) 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0.375 012.500.064 322.1440.030 061.0021.12637.520.287 89.592 µg·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% 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。

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

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 × 2.1 mm ID, 1.7 μm) 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 .  The linear response range was 0.375 0 12.50 µg·mL−1 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.

Key words:   
收稿日期:
相关功能
PDF(323KB) Free
打印本文
0
作者相关文章