高效液相色谱切换波长法同时测定辛夷鼻炎丸中4种成分的含量
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篇名: 高效液相色谱切换波长法同时测定辛夷鼻炎丸中4种成分的含量
TITLE:
摘要: 目的:建立同时测定辛夷鼻炎丸中升麻素苷、甘草苷、5-O-甲基维斯阿米醇苷、甘草酸铵含量的方法。方法:采用高效液相色谱切换波长法对A、B、C 3家企业共52批次辛夷鼻炎丸样品进行含量测定。色谱柱为Kromasil C18,流动相为乙腈-0.1%磷酸,流速为1.0 mL/min,检测波长为220 nm(升麻素苷、甘草苷、5-O-甲基维斯阿米醇苷)和250 nm(甘草酸铵),柱温为30 ℃,进样量为10 μL。结果:升麻素苷、甘草苷、5-O-甲基维斯阿米醇苷、甘草酸铵检测质量浓度线性范围分别为6.138~122.77 μg/mL(r=0.999 9)、2.502~50.03 μg/mL(r=0.999 9)、5.988~119.75 μg/mL(r=0.999 9)、12.788~255.76 μg/mL(r=0.999 9);精密度、稳定性和重复性试验的RSD均<2.0%(n=6);加样回收率分别为100.32%(RSD=0.58%,n=6)、100.24%(RSD=0.56%,n=6)、101.28%(RSD=0.91%,n=6)、101.48%(RSD=0.79%,n=6)。A企业的4种成分含量测定总值普遍高于B、C企业,其中甘草苷的差异尤为显著;B企业的升麻素苷含量高于A、C企业,而5-O-甲基维斯阿米醇苷却低于A、C企业;B企业甘草苷的含量均是离群值。结论:该方法操作简便、重复性好,可为辛夷鼻炎丸的质量控制提供参考。
ABSTRACT: OBJECTIVE: To establish the method for simultaneous determination of pim-O-glucosylcimifugin, liquiritin, 5-O- methylvisammioside and amonium glycyrrhizinate in Xinyi byan pills. METHODS: HPLC-switching wavelength method was used for content determination of 52 batches of Xinyi byan pills sample from enterprises A, B, C. The determination was performed on Kromasil C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid at the flow rate of 1.0 mL/min. The detection wavelengths were set at 220 nm (pim-O-glucosylcimifugin, liquiritin, 5-O-methylvisammioside) and 250 nm (amonium glycyrrhizinate). The column temperature was 30 ℃, and sample size was 10 μL. RESULTS: The linear ranges of prim-O-glucosylcimifugin, liquiritin, 5-O-methylvisammioside and amonium glycyrrhizinate were 6.138-122.77 μg/mL (r=0.999 9), 2.502-50.03 μg/mL (r=0.999 9), 5.988-119.75 μg/mL (r=0.999 9) and 12.788-255.76 μg/mL (r=0.999 9), respectively. RSDs of precision, stability and reproducibility tests were all lower than 2.0% (n=6). The recovery rate were 100.32% (RSD=0.58%,n=6), 100.24% (RSD=0.56%,n=6), 101.28% (RSD=0.91%,n=6) and 101.48% (RSD=0.79%,n=6), respectively. Total contents of 4 components in enterprise A were generally higher than enterprises B, C, among which the difference of liquiritin was significant; the content of prim-O-glucosylcimifugin in enterprise B was higher than enterprises A, C, while the content of 5-O-methylvisammioside was lower than enterprises A, C. The content of liquiritin in enterprise B was outlier. CONCLUSIONS: This method is simple, reproducible and can provide reference for quality control of Xinyi biyan pills.
期刊: 2018年第29卷第5期
作者: 黄莉莉,罗轶,吴桂凡,谢培德,张涛
AUTHORS: HUANG Lili,LUO Yi,WU Guifan,XIE Peide,ZHANG Tao
关键字: 辛夷鼻炎丸;升麻素苷;甘草苷;5-O-甲基维斯阿米醇苷;甘草酸铵;高效液相色谱法;切换波长法
KEYWORDS: Xinyi biyan pills; Pim-O-glucosylcimifugin; Liquiritin; 5-O-methylvisammioside; Amonium glycyrrhizinate; HPLC; Switching wavelength method
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