毛细管区带电泳法同时测定制马钱子中4种生物碱的含量  

Simultaneous Determination of Four Alkaloids in Processed Nux Vomica by Capillary Zone Electrophoresis

作　　者：张芳[1] 潘扬[1,2] 刘亮镜 

机构地区：[1]南京中医药大学药学院,江苏南京210029 [2]南京中医药大学江苏省中药炮制重点实验室,江苏南京210029 [3]芜湖市中医医院制剂科,安徽芜湖241000

出　　处：《药物生物技术》2011年第5期441-444,共4页Pharmaceutical Biotechnology

基　　金：南京中医药大学科技项目(重点培育)(No.09XPY03);2008年青蓝工程项目

摘　　要：建立了同时测定制马钱子中4种生物碱士的宁(S)、马钱子碱(B)、士的宁氮氧化物(SNO)和马钱子碱氮氧化物(BNO)含量的毛细管区带电泳法(CZE)。考察了缓冲溶液的种类、浓度和pH值以及分离电压等因素对分离结果的影响。以盐酸麻黄碱(EP)为内标,在缓冲溶液为40 mmol/L醋酸铵(以200 mmol/L醋酸溶液调pH 3.64)、分离电压25 kV及检测波长203 nm的优化条件下,7 min内即可实现分离测试。S、B、SNO和BNO分别在13.7～109.8μg/mL、13.4～107.5μg/mL、13.6～108.5μg/mL和3.3～106.2μg/mL范围内线性关系良好,相关系数分别为0.998 2、0.994 2、0.996 5和0.996 5;最低检出限分别为0.83、0.96、2.1和2.5μg/mL(信噪比为3);加标回收率分别为95.1%～102.5%、95.3%～102.0%、96.7%～102.9%和97.2%～104.2%,相对标准偏差3.75%、3.82%、3.55%和3.51%。A method for the simultaneous determination of strychnine,brucine, strychnine N-oxide and brucine N-oxide in processed nux vomica by capillary zone electrophoresis （CZE） was developed. The influences of type, concentration and pH value of the running buffer, and applied voltage on separation were investigated. Using ephedrine hydrochloride as an internal standard, under the conditions of 40 mmol/L ammonium （adjusting pH value 3.64 with 200 mmol/L acetic acid solution）, applied voltage of 25 kV and detection wavelength of 203 nm, the four alkaloids were separated and analyzed in 7 rain. The method was proved to be robust through verification of accuracy, precision and linearity. The calibration curves of S, B, SNO and BNO showed good linearity in the range of 13.7 - 109. 8 μg/mL,13.4 - 107.5 μg/mL, 13.6 - 108.5μg/mL and 3.3 - 106. 2 μg/mL, and the correlation coefficients were 0. 998 2,0. 9942,0. 9965 and 0. 9965 ,respectively. The limits of detection for S ,B ,SNO and BNO were 0. 83,0. 96,2. 1μg/mL and 2. 5 μg/mL （S/N = 3 ）. The addition recoveries of standards at three spiked levels were 95.1% -102.5% , 95.3% - 102. 0% , 96.7% - 102.9% and 97.2% - 104.2% with acceptable relative standard deviations of 3.75% ,3.82% ,3.55% and 3.51%.

关 键 词：毛细管区带电泳 制马钱子 士的宁 马钱子碱 士的宁氮氧化物 马钱子碱氮氧化物 

分 类 号：Q503[生物学—生物化学] R93[医药卫生—生药学]