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目的:心痛宁喷雾剂质量标准中,有对其有效成分阿魏酸和肉桂酸的含量测定要求,但为两套不同的方法。为节约检测时间和检测成本,本研究建立了以HPLC同时测定心痛宁喷雾剂中有效成分阿魏酸和肉桂酸含量的方法。方法:采用高效液相色谱法对有效成分进行分离并计算其含量,色谱条件为Phenomenex Luna C18(4.6 mm×150 mm,5μm)液相色谱柱,以乙腈-0.05%磷酸水溶液为流动相,梯度洗脱;检测波长290 mm,流速为1.0 m L·min-1,柱温30℃。选取1批心痛宁喷雾剂样品进行方法学验证试验,后对4批心痛宁喷雾剂样品按该方法进行含量测定。结果:空白干扰试验、精密度试验、稳定性试验、重复性试验、线性关系考察、加样回收率试验均符合方法学验证试验相关要求,RSD<3%。线性关系考察中阿魏酸、肉桂酸分别在0.025 16~0.276 76,0.010 4~0.114 4 mg·L-1有良好线性关系,r分别为1,0.999 5。两个组分均能达到基线分离,分离度>2。加样回收率试验中阿魏酸、肉桂酸的平均回收率分别为100.35%,101.93%。结论:本方法简便、准确、重复性好,可作为该制剂质量控制的方法,且可达到节约检测时间和检测成本的目的。该方法对于中成药质量标准中多组分含量测定方法的建立具有借鉴意义。
OBJECTIVE: In the quality standard of Xintongning Spray, there are requirements for the content determination of ferulic acid and cinnamic acid, the effective components of which are two sets of different methods. In order to save testing time and testing costs, this study established a method for the simultaneous determination of ferulic acid and cinnamic acid, the active ingredients of Xintongning Spray by HPLC. Methods: The active constituents were separated and calculated by HPLC. The chromatographic conditions were as follows: Phenomenex Luna C18 (4.6 mm × 150 mm, 5 μm), acetonitrile-0.05% phosphoric acid solution as mobile phase, gradient The detection wavelength was 290 mm and the flow rate was 1.0 m L · min-1. The column temperature was 30 ℃. A batch of Xintongning spray samples was selected for verification of methodological validation. Four batches of Xintongning spray samples were determined according to the method. Results: Blank interference test, precision test, stability test, repeatability test, linear relationship test and sample recovery test all met the requirements of the methodological validation test with RSD <3%. There was a good linear relationship between ferulic acid and cinnamic acid in the range of 0.025 16 ~ 0.276 76 and 0.010 4 ~ 0.114 4 mg · L -1, respectively, with r values of 1, 0.9999. Baseline separation was achieved for both components with resolution> 2. The average recoveries of ferulic acid and cinnamic acid in the recovery test were 100.35% and 101.93%, respectively. Conclusion: The method is simple, accurate and reproducible. It can be used as a method for quality control of the preparation and can save time and cost. The method has reference significance for the establishment of the method for determining the content of multi-component in the quality standard of Chinese patent medicines.