HPLC-ELSD法测定龙泽熊胆胶囊中牛磺熊去氧胆酸和牛磺鹅去氧胆酸的含量
Determination of taursodeoxycholic acid and taurchenodeoxycholic acid in Longze Xiongdan capsules by HPLC-ELSD
乔莉 1陈正东 1陈馥 1简淑仪 1黄俊忠 1黄悠雯 1刘潇潇1
作者信息
摘要
目的:以牛磺熊去氧胆酸和牛磺鹅去氧胆酸为指标,建立龙泽熊胆胶囊中熊胆粉的含量测定方法.方法:采用高效液相色谱串联蒸发光检测器,色谱柱为ChromCore AQ C18(4.6 mm ×250 mm,5 μm),乙腈(A)-5 mmol·L-1 醋酸铵溶液(B)为流动相,梯度洗脱(0～40 min,25％A;40～50 min,25％A→29％A;50～80 min,29％A;80～100 min,29％A→40％A),流速 1.0 mL·min-1,柱温 30 ℃,ELSD 漂移管温度 110℃,氮流量2.5L·min-1.结果:牛磺熊去氧胆酸进样量在1.069～9.57μg内、牛磺鹅去氧胆酸进样量在0.740 46～7.404 64 μg内,进样量的对数与峰面积的对数呈良好的线性关系;仪器精密度、重复性、稳定性试验的RSD＜2.0％;经低、中、高3个浓度的准确度试验考察,牛磺熊去氧胆酸的回收率为95.2％～97.7％,牛磺鹅去氧胆酸的回收率为91.9％～95.9％.测定样品42批次,牛磺熊去氧胆酸和牛磺鹅去氧胆酸的含量分别为0.18～0.43、0.10～0.44 mg·粒-1.结论:本法适用于龙泽熊胆胶囊中熊胆粉的质量控制,可为完善龙泽熊胆胶囊的质量标准提供科学的依据.
Abstract
Objective:To establish a method for determining the content of bear bile powder in Longze Xiongdan capsules with taursodeoxycholic acid(TUDCA)and taurchenodeoxycholic acid(TCDCA)as indexes.Methods:HPLC series evaporation photodetector was adopted on Chrom Core AQ C18 column(4.6 mm ×250 mm,5 μm),with the mobile phase comprising of acetonitrile(A)and 5 mmol·L-1 ammonium acetate solution(B)in a gra-dient elution(0-40 min,25％A;40-50 min,25％A→29％A;50-80 min,29％A;80-100 min,29％A→40％A)at the flow rate of 1.0 mL·min-1:The column temperature was 30 ℃.The ELSD was used,of which the drift tube temperature was 110 ℃ and the flow rate of carrier gas(N2)was 2.5 L·min-1.Results:In the ranges of 1.069-9.57 μg and 0.740 46-7.404 64 μg,logarithms of the injected amount of TUDCA and TCDCA pres-ented good linear relationships with logarithms of the peak area,respectively.The RSDs of precision,repeatability and stability tests were all lower than 2.0％.At three concentration levels the recoveries of TUDCA and TCDCA were 95.2％-97.7％and 91.9％-95.9％,respectively.Samples of 42 batches showed that the contents of TUDCA and TCDCA were 0.18-0.43 and 0.10-0.44 mg·granule-1,respectively.Conclusion:This method can be used for the quality control of bear bile powder in Longze Xiongdan capsules,thus provides a scientific basis for improving its quality standard.
关键词
高效液相色谱-蒸发光散射检测器/龙泽熊胆胶囊/熊胆粉/牛磺熊去氧胆酸/牛磺鹅去氧胆酸Key words
HPLC-ELSD/Longze Xiongdan capsules/bear bile powder/taursodeoxycholic acid/taurchenodeoxy-cholic acid引用本文复制引用
出版年
2024
NETL
NSTL
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