固相萃取-超高效液相色谱法同时测定肉蔻四神丸中3种有效成分含量  

Simultaneous Determination of Three Alkaloids in Roukousishen Pills by SPE-UPLC

作　　者：刘永利[1] 李冬梅[1] 袁浩[1] 张淼[1] 冯丽[1] 

机构地区：[1]河北省药品检验所,石家庄050011

出　　处：《中国药学杂志》2011年第22期1753-1755,共3页Chinese Pharmaceutical Journal

摘　　要：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。ABSTRACT ： OBJECTIVE To establish a new UPLC method for the determination of morphine, codeine and papaverine in Roukou- sishen pills. METHODS The extract of the sample were passed through a SPE column tO achieve good chromatographic performance. The separation was performed on a Waters Acquity ClS BEH column （2. 1 mmХ 100mm, 1.7μm） with gradient elution using acetoni- trile and 0. 1% phosphoric acid at a flow rate of 0.4 mL·min^-1. The detection wavelengths were set at 210 nm for morphine and code- ine phosphate, and 251 nm for papaverine hydrochloride. The column temperature was 30 ℃. RESULTS Under the optimized condi- tions, there was good linear relationship between the mass concentrations and the peak areas of morphine, codeine phosphate and papav- erine hydrochloride in the range of 0. 514 0 - 10. 28, 0. 254 5 -5. 090 and 0. 050 5 - 1. 010μg ·mL^-1 with a correlation coefficient of 0. 999 9. The average recoveries were 99. 51%, 98. 18% and 100. 7%, respectively. CONCLUSION The method is accurate,sen- sitive,highly reproducible and suitable for the quality control of Roukousishen pills.

关 键 词：超高效液相色谱法 固相萃取 肉蔻四神丸 吗啡 可待因 罂粟碱 

分 类 号：R917[医药卫生—药物分析学]