高效液相色谱法测定牛黄解毒片中胆酸和猪去氧胆酸的含量及其质量分析
陈小红,陈广云
淮安市食品药品检验所,江苏淮安 223001
Determination and quality analysis of cholic acid and porcine deoxycholic acid in Niuhuang Jiedu Tablets by high performance liquid chromatography
CHEN Xiaohong, CHEN Guangyun
Huaian Institute for Food and Drug Control, Huaian 223001, China
摘要:建立高效液相色谱法测定牛黄解毒片中胆酸和猪去氧胆酸的含量的方法,分析不同厂家、不同批次牛黄解毒片中这两种成分的差异。选用Welch Ultimate LP-C18柱(250 mm×4.60 mm, 5?m)为分离柱,流动相为甲醇-乙腈-0.1%甲酸溶液(体积比为63∶17∶20),流量为0.8 mL/min,柱温为30℃,蒸发光散射检测器。胆酸、猪去氧胆酸质量分别在0.511 5~5.115 1?g、0.487 5~4.874 7?g范围内与色谱峰面积对数具有良好的线性关系,相关系数分别为0.999 8、0.999 9,方法检出限分别为0.09、0.09?g。胆酸、猪去氧胆酸测定结果的相对标准偏差分别为0.4%、0.7%(n=6),样品加标回收率分别为96.89%~99.60%、96.85%~98.60%。不同厂家、不同批次牛黄解毒片中胆酸和猪去氧胆酸的总量存在较大差异,其含量为0.217 4~0.721 6 mg/片。该方法简单,重复性好,结果准确,适用于牛黄解毒片中胆酸和猪去氧胆酸含量的测定。
Abstract:A high performance liquid chromatography was established for the determination of cholic acid and porcine deoxycholic acid in Niuhuang Jiedu Tablets, the di ?erences of these two components in Niuhuang Jiedu Tablets from di ?erent manufacturers and batches were analyzed. Welch ultimate LP-C18 column(250 mm×4.6 mm, 5 μm) was selected as the separation column, the mobile phase was methanol-acetonitrile-0.1% formic acid solution (volume ratio was 63∶17∶20), the ?ow rate was 0.8 mL/min, the column temperature was 30 ℃and the detector was an evaporative light scattering detector. The quality of cholic acid and porcine deoxycholic acid has a good linear relationship with the logarithm of chromatographic peak area in the range of 0.511 5-5.115 1μg and 0.487 5-4.874 7 μg, and the correlation coe?cients were 0.999 8 and 0.999 9, the detection limits were 0.09, 0.09μg, respectively. The relative standard deviations of cholic acid and porcine deoxycholic acid were 0.4%, 0.7% (n=6), the recoveries of spiked samples were 96.89%-99.60%, 96.85%-98.60%, respectively. There were great di?erences in the total amount of cholic acid and porcine deoxycholic acid in Niuhuang Jiedu Tablets from di ?erent manufacturers and batches, and the content was 0.217 4-0.721 6 mg/tablet. The method is simple, reproducible and accurate, which is suitable for the determination of cholic acid and porcine deoxycholic acid in Niuhuang Jiedu Tablets.
关键词:牛黄解毒片;高效液相色谱法;胆酸;猪去氧胆酸;聚类分析
Keywords:Niuhuang Jiedu Tablets; high performance liquid chromatography; cholic acid; porcine deoxycholic acid;cluster analysis
本文引用格式:
陈小红,陈广云.高效液相色谱法测定牛黄解毒片中胆酸和猪去氧胆酸的含量及其质量分析[J].化学分析计量,2022,31(4):45.
CHEN Xiaohong,CHEN Guangyun. Determination and quality analysis of cholic acid and porcine deoxycholic acid in Niuhuang Jiedu Tablets by high performance liquid chromatography[J]. Chemical analysis and meterage,2022,31(4):45.
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