[参附注射液中乌头碱、次乌头碱和新乌头碱的测定]
[Determination of aconitine, hypaconitine and mesaconitine in Shenfu injection].
作者信息
Zhang Pan-Pan, Zhang Jun-Zhen, Wang Zhao-Hong, Lu Yong-Jiang, Jiang Ye
机构信息
School of Pharmacology, Hebei Medical University, Shijiazhuang 050017, China.
出版信息
Zhongguo Zhong Yao Za Zhi. 2013 May;38(10):1521-5.
To establish a method for the content determination of indexes for measuring aconitic compounds contained in Shenfu injection, in order to provide basis for the evaluation of the curative effect of monkshood in Shenfu injection. The sample were purified and enriched with HF-LPME. ACQUITY UPLC BEH C18 column (2.1 mm x 50 mm, 1.7 microm) was adopted and eluted with a gradient program, with acetonitrile-10 mmol x L(-1) NH4HCO3 (pH 10) as the mobile phases. The flow rate was 0.45 mL x min(-1). The content was determined with ESI and MRM. The results showed that aconitine, hypaconitine and mesaconitine showed a good linear relationship, with r > 0.999, within the range of 0.1-100 ng x L(-1). The recoveries were detected to be 100.1%, 97.4%, 97.5%, with RSD being 1.2%, 1.1%, 1.5%, respectively. This method was used to prove the safety of Shenfu injection, and provide scientific basis for correct evaluation of curative effect of monkshood, as well as a reliable, simple and practical means for quality control of monkshood-containing Chinese materia medica preparations.
建立参附注射液中乌头类化合物测定指标的含量测定方法，为评价参附注射液中附子的疗效提供依据。样品采用中空纤维液相微萃取进行净化和富集。采用ACQUITY UPLC BEH C18色谱柱（2.1 mm×50 mm，1.7 µm），以乙腈-10 mmol·L⁻¹ NH₄HCO₃（pH 10）为流动相进行梯度洗脱。流速为0.45 mL·min⁻¹。采用电喷雾离子化和多反应监测模式测定含量。结果表明，在0.1～100 ng·L⁻¹范围内，乌头碱、次乌头碱和新乌头碱呈现良好的线性关系，r＞0.999。回收率分别为100.1%、97.4%、97.5%，相对标准偏差分别为1.2%、1.1%、1.5%。该方法用于证明参附注射液的安全性，为正确评价附子的疗效提供科学依据，也为含附子中药制剂的质量控制提供了可靠、简便、实用的手段。
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