摘要
目的 建立高效液相色谱-蒸发光散射检测法(HPLC-ELSD)测定中乌宁碱的含量。方法 使用Gemini C18 110A(4.6 mm×150 mm,5 μm)色谱柱,以甲醇-0.1%三氟乙酸(25:75)为流动相,流速为0.6 mL·min-1,使用Alltech ELSD 2000ES检测器,漂移管温度90 ℃,气体流速2.3 L·min-1。结果 中乌宁碱在0.40~0.60 mg·mL-1内峰面积的对数与浓度的对数呈良好线性关系(r=0.999 6);进样精密度RSD为0.04%(n=5);重复性试验RSD为0.7%(n=6);日内精密度RSD为0.4%;日间精密度RSD为0.6%;平均回收率为101.0%(RSD=1.1%;n=9)。结论 本法专属、简便、准确,适用于中乌宁碱的含量测定。
Abstract
OBJECTIVE To establish an HPLC-ELSD method for determination of mesaconine.METHODS Gemini C18 110A column (4.6 mm×150 mm,5 μm) was adopted with the mobile phase consisting of methanol-0.1%TFA (25:75) at the flow rate of 0.6 mL·min-1. The detector was Alltech ELSD 2000ES, with the drift tube temperature of 90 ℃ and the airflow velocity of 2.3 L·min-1. RESULTS Under this conditions, mesaconine and the related substances were well separated. The linear range of mesaconine was 0.40-0.60 mg·mL-1 (r=0.999 6). RSD of injection precision and repeatability test were 0.04% (n=5) and 0.7% (n=6), the intra day and inter day precision RSD were 0.4% and 0.6%, respectively. The average recovery was 101.0% (RSD=1.1%, n=9). CONCLUSION The established method was specific, simple, accurate, and suitable for determination of mesaconine.
关键词
高效液相色谱-蒸发光散射检测法 /
中乌宁碱 /
含量测定
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Key words
HPLC-ELSD /
mesaconine /
content determination
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刘涛红, 刘秀秀, 晁若冰.
高效液相色谱-蒸发光散射检测法测定中乌宁碱的含量[J]. 中国药学杂志, 2016, 51(17): 1459-1461 https://doi.org/10.11669/cpj.2016.17.005
LIU Tao-hong, LIU Xiu-xiu, CHAO Ruo-bing.
Determination of Mesaconine by HPLC-ELSD Method[J]. Chinese Pharmaceutical Journal, 2016, 51(17): 1459-1461 https://doi.org/10.11669/cpj.2016.17.005
中图分类号:
R917
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参考文献
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脚注
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