首页|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

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

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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。
Determination of taursodeoxycholic acid and taurchenodeoxycholic acid in Longze Xiongdan capsules by HPLC-ELSD
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.

HPLC-ELSDLongze Xiongdan capsulesbear bile powdertaursodeoxycholic acidtaurchenodeoxy-cholic acid

乔莉、陈正东、陈馥、简淑仪、黄俊忠、黄悠雯、刘潇潇

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广东省药品检验所,广州 510663

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

广东省中医药局课题

20221056

2024

中国药品标准
国家药典委员会

中国药品标准

影响因子:0.372
ISSN:1009-3656
年,卷(期):2024.25(1)
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