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反相离子对色谱法测定青风藤中青藤碱的含量
王慧,叶卿,赵亮,田文君,张国庆*
0
(第二军医大学东方肝胆外科医院药材科,上海 200438)
摘要:
目的建立离子对色谱法测定青风藤中青藤碱的含量。方法使用Eclipse Plus C18柱 (4.6 mm×250 mm,5 μm);乙腈磷酸盐缓冲液(0.03 mol/L磷酸二氢钾和0.03 mol/L庚烷磺酸钠,磷酸调节pH值至4.0)=1882为流动相,流速1.0 ml/min,柱温40℃,检测波长262 nm。结果青藤碱在0.025~0.5 mg/ml(r=1.000)范围内呈良好的线性关系。最低检测限为2.5 μg/ml,低、中、高3个浓度的日内精密度RSD分别为0.62%、0.35%、0.60%,日间精密度RSD为1.54%、0.70%、0.45%。平均回收率99.9%(RSD=2.9%,n=6),均符合分析要求。结论该方法简单快捷,结果准确,适用于测定青风藤中青藤碱的含量。
关键词:  青风藤  青藤碱  反相离子对色谱法  含量测定
DOI:10.3724/SP.J.1008.2010.0193
投稿时间:2009-10-12修订日期:2010-01-06
基金项目:
Reversed-phase ion-pair chromatography in determination of sinomenine contents in Sinomenium acutum
WANG Hui, YE Qing, ZHAO Liang, TIAN Wen-jun, ZHANG Guo-qing*
(Department of Pharmacy, Eastern Hepatobiliary Surgery Hospital, Second Military Medical University, Shanghai 200438, China)
Abstract:
ObjectiveTo establish a reversed-phase ion-pair chromatography (RP-IPC) method for determination of sinomenine content in Sinomenium acutum. MethodsThe IPC method was established using a column of Eclipse Plus C18 (4.6 mm×250 mm, 5 μm) with a mobile phase of acetonitrile and buffer phosphate (0.03 mol/L potassium dihydrogen phosphate and 0.03 mol/L sodium heptane sulfonic acid,adjusted to pH 4.0 by phosphoric acid)1882.The flow rate was 1.0 ml/min; the detection wavelength was set at 262 nm, and the temperature was at 40℃. ResultsThe linearity was obtained over a concentration range of 0.025-0.5 mg/ml(r=1.000). The low limit of detection was 2.5 μg/ml. The intra-day precisions of low, medium, and high concentrations of sinomenine were 1.54%, 0.70%, and 0.45%, and the inter-day precisions were 1.54%,0.70%, and 0.45%, respectively.The average recovery was 99.9%(RSD=2.9%, n=6), which met the requirement for analysis. Conclusion The present method is simple, fast, and accurate; it is suitable for determination of sinomenine content in Sinomenium acutum.
Key words:  Sinomenium acutum  sinomenine  reversed phase ion pair chromatography  determination