HPLC测定二巯丁二酸的有关物质

乐健 王麟达 陈桂良 洪战英

中国药学杂志 ›› 2011, Vol. 46 ›› Issue (13) : 1030-1033.

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PDF(643 KB)
中国药学杂志 ›› 2011, Vol. 46 ›› Issue (13) : 1030-1033.
论著

HPLC测定二巯丁二酸的有关物质

  • 乐健1,王麟达1,陈桂良1,洪战英2*
作者信息 +

Determination of Related Substances in Dimercaptosuccinic Acid by HPLC

  • LE Jian1,WANG Lin-da1,CHEN Gui-liang1,HONG Zhan-ying2*
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摘要

目的 建立二巯丁二酸中有关物质的HPLC测定方法方法 色谱柱为Ultimate XB-C18(4.6 mm×150 mm,5 μm);流动相A:硫酸氢四丁基铵磷酸盐溶液(含硫酸氢四丁基铵3.2 g·L-1、磷酸二氢钠6.5 g·L-1和乙二胺四乙酸二钠0.09 g·L-1)-甲醇(85∶15),流动相B:甲醇;流速:1.0 mL·min-1;检测波长220 nm;线性梯度洗脱:0 min,100%A;10 min,100%A;20 min,80%A;50 min,80%A。结果 二巯丁二酸与丁炔二酸、各杂质峰之间分离良好。二巯丁二酸在14.0~112.0 μg·mL-1内线性良好,r=0.999 3,检测限为1.8 μg·mL-1;丁炔二酸在10.3~82.3 μg·mL-1内线性良好,r=1.000 0,检测限为0.4 μg·mL-1,丁炔二钠的平均加样回收率为98.3%。结论方法专属性强、准确度高,适合测定二巯丁二酸的有关物质。

Abstract

OBJECTIVE To establish an HPLC method for determination of related substances in dimercaptosuccinic acid. METHODS An Ultimate XB-C18(4.6 mm×150 mm,5 μm) column was applied. Mobile phase A was tetrabutylammonium bisulfate phosphate solution containing tetrabutylammonium bisulfate 3.2 g·L-1, potassium dihydrogen phosphate 6.5 g·L-1 and disodium edenate 0.09 g·L-1, mobile phase B was meathanol. Gradient elution program: 0 min,100%A;10 min,100%A;20 min,80%A;50 min,80%A. The flow rate was 1.0 mL·min-1. Detection wavelength was set at 220 nm. RESULTS The linear range of dimercaptosuccinic acid was 14.0-112.0 μg·mL-1 (r=0.999 3),limit of detection was 1.8 μg·mL-1. The linear range of acetylenedicarboxylic acid was 10.3-82.3 μg·mL-1 (r=1.000 0),limit of detection was 0.4 μg·mL-1,while the average recovery was 98.3%. CONCLUSION This method proved to be specific,accurate and suitable for determining the related substances in dimercaptosuccinic acid.

关键词

二巯丁二酸 / 丁炔二酸 / 高效液相色谱法 / 有关物质 / 梯度洗脱

Key words

dimercaptosuccinic acid / acetylenedicarboxylic acid / HPLC / related substances / gradient elution

引用本文

导出引用
乐健 王麟达 陈桂良 洪战英. HPLC测定二巯丁二酸的有关物质[J]. 中国药学杂志, 2011, 46(13): 1030-1033
LE Jin;WNG Lin-d;CHEN Gui-ling;HONG Zhn-ying. Determination of Related Substances in Dimercaptosuccinic Acid by HPLC[J]. Chinese Pharmaceutical Journal, 2011, 46(13): 1030-1033

参考文献


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