HPLC-ELSD测定胆益宁片中甘氨猪去氧胆酸和甘氨鹅去氧胆酸含量

马若飞; 陈勇; 陈碧莲

doi:10.13748/j.cnki.issn1007-7693.2017.07.019

HPLC-ELSD测定胆益宁片中甘氨猪去氧胆酸和甘氨鹅去氧胆酸含量

Determination of Glycohyodeoxycholic Acid and Glycochenodeoxycholic Acid in Danyining Tablet by HPLC-ELSD

摘要

摘要: 目的建立HPLC-ELSD测定胆益宁片中的甘氨猪去氧胆酸和甘氨鹅去氧胆酸的含量测定方法。方法采用WelchUltimate Plus C₁₈色谱柱（250 mm×4.6 mm，5 μm），流动相：乙腈-0.1%甲酸溶液（40： 60），柱温： 35℃，流速： 1.0 mL·min^-1，检测器为ELSD6000型蒸发光散射检测器，漂移管温度为105℃，氮气流速为2.5 L·min^-1。结果甘氨猪去氧胆酸和甘氨鹅去氧胆酸分别在0.206~3.090 μg（r=0.999 5）和0.180~2.693 μg（r=0.999 4）内呈良好的线性，平均加样回收率分别为99.54%（RSD=0.99%）和100.58%（RSD=1.70%）。结论该方法简便、准确、重复性好，可用于胆益宁片的质量控制。

Abstract: OBJECTIVE To establish a method for the simultaneous determination of glycohyodeoxycholic acid and glycochenodeoxycholic acid in Danyining tablet by HPLC-ELSD.METHODS The analysis was performed on Welch Ultimate Plus C₁₈(250 mm×4.6 mm,5 μm),the mobile phase consisted of acetonitrile and 0.1% formic acid (40:60).The flow rate was 1.0 mL·min^-1.ELSD6000 was used as the detector,the drift tube temperature was 105℃ and the nitrogen flow rate was 2.5 L·min^-1.RESULTS Glycohyodeoxycholic acid and glycochenodeoxycholic acid had good linear relationships in the ranges of 0.206-3.090 μg (r=0.999 5) and 0.180-2.693 μg (r=0.999 4),respectively.The average recoveries were 99.54%(RSD=0.99%) and 100.58%(RSD=1.70%),respectively.CONCLUSION The method is simple,accurate with good repeatability,which can be used for the quality control of Danyining tablet.

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