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机构地区:[1]宁波市急救中心,浙江宁波315020 [2]宁波市药品检验所,浙江宁波315004
出 处:《中国卫生检验杂志》2016年第8期1105-1106,共2页Chinese Journal of Health Laboratory Technology
摘 要:目的建立足光散中氧化苦参碱的高效液相色谱(HPLC)定量方法。方法样品前处理采用氨水碱化,三氯甲烷超声提取的方法。高效液相色谱法使用Inertsil ODS-SP色谱柱(4.6 mm×150 mm,5μm),以乙腈-0.1%磷酸(20∶80,V/V,加三乙胺调节p H值至7.8)为流动相,流速为1.0 ml/min,柱温为35℃,检测波长为210 nm,进样量为10μl。结果氧化苦参碱的浓度为46.6μg/ml^466.0μg/ml时,线性关系良好,线性方程为y=109.66x+0.55,相关系数(r)为0.999 8。氧化苦参碱精密度试验测得的相对标准偏差(RSD)为0.1%(n=6);加标回收率实验测得的平均回收率为99.0%(n=6),RSD为0.4%。结论本方法简便有效,稳定可靠,可用于足光散中氧化苦参碱的质量控制。Objective A high performance liquid chromatography method( HPLC) was developed to quantify oxymatrine in Zuguangsan. Methods Sample was alkalized by ammonia and extract with ultrasound and chloroform. The HPLC method was carried out with Inertsil ODS- SP column and the mobile phase of acetonitrile- 0. 1% phosphoric acid( 20∶80,V / V,adjusting p H to 7. 8 with triethylamine). The flow rate was 1. 0 ml / min. The temperature was 35℃. The detection wavelength was set at 210 nm,and the sample volume was set at 10 μl. Results The good linearity was obtained when the concentration of oxymatrine was among 46. 6 μg / ml- 466. 0 μg / ml,and the its equation was y = 109. 66 x + 0. 55,with the correlation coefficients of 0. 999 8. The relative standard deviation( RSD) of the fine density test of oxidized matrine was 0. 1%( n = 6). The average recovery was 99. 0%( n = 6) with RSD of 0. 4%. Conclusion This method was simple,steady for the determination of oxymatrine in Zuguansan.
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