目的 用在线基质消除-离子色谱系统直接进样测定硫酸氢氯吡咯雷中的痕量相转移催化剂四乙基溴化铵的残留。方法 采用Dionex IonPac NG1柱为样品预处理柱,20 mmol·L-1甲烷磺酸(MSA)为洗脱液,将所需分析的痕量四乙基溴化铵从硫酸氢氯吡格雷基质中分离出来,被分析组分通过Dionex CG17进行浓缩,再以Dionex IonPacCS17为分析柱,含35%乙腈(体积比)的5 mmol·L-1MSA为淋洗液进行分离,非抑制性电导检测器进行检测。结果 方法重复性良好,回收率在97.8%~103.3%之间,最低检出为0.2 μg·mL-1,在0.4~10 μg·mL-1内线性关系良好。结论 建立了痕量阳离子在线基质消除-离子色谱测定的方法,在药物的阳离子残留控制中可推广应用。
Abstract
OBJECTIVE To establish a method of on-line matrix elimination together with ion chromatographic for determination of residual tetraethylammonium bromibde(TEAB) which acts as phase transfer catalyst in clopidogrel sulfate. METHODS An ion excluding column Dionex IonPac NG1 was used for the separation of TEAB from clopidogrel sulfate, using 20 mmol·L-1 MSA as eluent. A pre-concentration column Dionex CG17 was used to enrich the trace TEAB. After being switched to analytical system, the separation was performed on Dionex ICS3000 using Dionex IonPac CS17 as analytical column, and suppressor was not required. 5 mmol·L-1 MSA containing 35% acetonitrile was used as mobile phase. RESULTS The RSDs of retention time and peak area were good. The recoveries of TEAB were between 97.8%-103.3%. The calibration curves of analytes were linear in the range between 0.4 and 10.0 μg·mL-1. The limit of detection reached 0.2 μg·mL-1. CONCLUSION This method can be applied to detect trace kation in pharmaceutical chemicals.
关键词
硫酸氢氯吡格雷 /
四乙基溴化铵 /
离子色谱 /
在线基质消除 /
相转移催化剂
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Key words
clopidogrel sulfate /
tetraethyl ammonium bromide /
ion chromatography /
on-line matrix elimination /
phase transfer catalyst
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中图分类号：
R917
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参考文献
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脚注
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基金
浙江省公益技术应用研究(分析测试)项目资助(2016C37020)
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