世界中医药

作者	单位
陈世雄1，翟青1，袁平川2，柳春燕2	1 安徽省芜湖市第二人民医院药剂科,芜湖,241000 2 皖南医学院药物研发中心,芜湖,241000

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中文摘要:

目的:通过超高效液相色谱法分析蒲地蓝消炎口服液的化学成分。方法:采用Waters C18色谱柱(型号为Xbridge),该色谱柱填料颗粒直径为5 μm,色谱柱的长度为250 mm,色谱柱内经为4.6 mm,柱温30 ℃。进样量为10 μL,流动相采用乙腈(A相)和0.2%磷酸水溶液(B相)的二元体系进行梯度洗脱,超高效液相色谱法方法严谨性考察,包括线性关系、精密度、重复性、稳定性和加样回收试验考察,基于超高效液相色谱法方法具有严谨性的前提下,对蒲地蓝消炎口服液中成分的含量进行测定。结果:1)线性考察结果显示回归方程、相关系数和线性范围分别是:结果表明黄芩苷在90.59~1 449.36 μg范围内与峰面积呈良好的线性关系,其回归方程为Y=17 465X+22 879(r=0.999 9);菊苣酸得回归方程Y＝39 728X+15 520(r＝0.999 8),在5.48~54.85 μg范围内与峰面积积分值呈良好的线性关系。2)精密度试验结果显示,黄芩苷峰面积的RSD＝0.18%,菊苣酸峰面积的RSD=0.16%,结果表明超高效液相仪器精密度良好。3)稳定性试验结果显示黄芩苷峰面积的RSD＝0.96%,菊苣酸峰面积的RSD=0.87%,符合色谱峰相对峰面积的RSD<3%则说明稳定性良好,提示蒲地蓝消炎口服液供试品溶液24 h内稳定性良好。4)重复性试验研究结果显黄芩苷峰面积的RSD＝0.99%,菊苣酸峰面积的RSD=1.06%,符合色谱峰相对峰面积的RSD<3%表示重复性良好,提示蒲地蓝消炎口服液供试品溶液的重复性良好。5)加样回收试验结果显示黄芩苷对照品溶液、菊苣酸对照品溶液平均回收率分别为105.887%、99.033%,RSD分别为1.03%、1.11%,提示高相液相检测方法所测加样回收率结果可靠。6)3个不同批次的蒲地蓝消炎口服液中黄芩苷成分和菊苣酸成分的含量差异无统计学意义,另外3批蒲地蓝消炎口服液的相似度检测结果也比较相近。结论:超高效液相色谱法的操作简单,方法严谨性强,可作为蒲地蓝消炎口服液质量控制的有效方法,而不同批次蒲地蓝消炎口服液中有效成分含量未见明显差异,且相似度高。

English Summary:

To analyze the chemical composition of Pudilan Xiaoyan oral liquid by ultra-high performance liquid chromatography.Methods:Waters C18 column (model Xbridge) was used.The diameter of the column filler particle was 5 μm，and the length of the column was 250 mm.The inner diameter of the column was 4.6 mm，and the temperature of the column was 30 °C.The sample intake was 10 μL.The flow phase used a binary system of acetonitrile (phase A) and 0.2 % phosphate aqueous solution (phase B) for gradient elution.The ultra-high performance liquid chromatography method was rigorous，including linear relationship，precision，repeatability，stability，and sample recovery.Based on the rigorous method of ultra-high performance liquid chromatography，the content of Pudilan Xiaoyan oral liquid was determined.Results:1) The linear results showed that the regression equation，the correlation coefficient，and the linear range were：the results showed that baicalin had a good linear relationship with the peak area in the range of 90.59 to 1 449.36 μg.Its regression equation was Y=17 465 X+22 879 (r=0.999 9); The regression equation Y=39 728X+15 520 (r=0.999 8) of Chicory acid had a good linear relationship with the peak area integral value in the range of 5.48 to 54.85 μg.2) The results of the precision test showed that the RSD=0.18 in the peak area and the RSD=0.16% in the peak area of Chicory acid.The results showed that the ultra-high liquid phase instrument had good precision.3) The stability test results showed that the RSD=0.96 in the peak area of Astragalin，and the RSD=0.87 % in the peak area of Chicory acid，which was in line with the RSD<3% in the peak area of the chromatographic peak，which showed good stability，suggesting that the stability of the Pudilan Xiaoyan oral liquid for the test solution was good within 24 h.4) The results of repetitive experiments showed that the RSD=0.99 in the peak area of scutellaria，the RSD=1.06 % in the peak area of Chicory，and the RSD<3% in the relative peak area of the peak of the spectrum，which indicated good repeatability，suggesting that the Pudilan Xiaoyan oral liquid had good repeatability for trial solution.5) The results of the sample recovery test showed that the average recovery rates of baicalin reference solution and Chicory acid reference solution were 105.887 % and 99.033 %，respectively，and RSD was 1.03 % and 1.11 %，respectively.It was suggested that the sample recovery rate measured by high phase liquid detection method was reliable.6) The content of baicalin and Chicory acid in 3 different batches of Pudilan Xiaoyan oral liquid was not significantly different，and the similarity test results of three batches of Pudilan Xiaoyan oral liquid were similar.Conclusion:The high performance liquid chromatography (HPLC) method is simple and strict.It can be used as an effective method to control the quality of Pudilan Xiaoyan oral liquid，but there is no significant difference in the content of active ingredients in different batches of Pudilan Xiaoyan oral liquid，and the similarity is high.

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