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目的:建立测定猪胆粉中主要胆汁酸类成分的HPLS-ELSD法,并对样品的全轮廓色谱图进行化学计量学分析。方法:采用SB-C_(18)色谱柱(4.6 mm×250 mm,5μm),柱温为40℃,流动相为0.2%甲酸水溶液-乙腈,梯度洗脱,流速1.0 m L·min~(-1);ELSD漂移管温度为110℃,氮气流量为2.8 L·h~(-1),增益为1。使用COW法校正样品的色谱峰,并对数据进行聚类分析和主成分分析。结果:有2批样品未检出甘氨猪去氧胆酸和甘氨鹅去氧胆酸,另外20批样品的甘氨猪去氧胆酸和甘氨鹅去氧胆酸的含量分别在6.4%~36.5%和4.5%~27.0%之间。化学计量学分析结果表明,自制样品与对照药材图谱更接近,而与市售样品差异较大。结论:该法适合从定性和定量的角度对猪胆粉进行质量评价与控制。
OBJECTIVE: To establish an HPLS-ELSD method for the determination of major bile acids in porcine bile powder and to perform chemometric analysis of the whole contour chromatogram of the sample. Methods: The mobile phase consisted of 0.2% formic acid in acetonitrile and gradient elution at a flow rate of 1.0 mL · min ~ (-1) on a SB-C 18 column (4.6 mm × 250 mm, 5 μm) 1). The temperature of the ELSD drift tube was 110 ℃, the nitrogen flow rate was 2.8 L · h -1 and the gain was 1. The COW method was used to calibrate the chromatographic peaks of the samples, and the data were clustered and principal component analysis. Results: Glycyrrhizin and glycochenodeoxycholic acid were not detected in two batches of samples, and the contents of glycine deoxycholic acid and glycochenodeoxycholic acid in 20 batches of samples were 6.4% ~ 36.5% and 4.5% ~ 27.0%. The results of stoichiometric analysis showed that the self-made samples were more similar to the reference drug samples, but different from the commercial samples. Conclusion: This method is suitable for quality evaluation and control of porcine bile powder from qualitative and quantitative point of view.