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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 IonPac CS17为分析柱,含35%乙腈(体积比)的5 mmol·L~(-1)MSA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0.2μg·mL~(-1),在0.4~10μg·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。
OBJECTIVE To determine the trace of tetraethylammonium bromide (TRAB) in the presence of trace matrix phase transfer catalyst in on-line matrix elimination-ion chromatography system. Methods Dionex IonPac NG1 column was used as sample pretreatment column and 20 mmol·L -1 methanesulfonic acid (MSA) as eluent. The trace amount of tetraethylammonium bromide Gray matrix. The analytes were concentrated by Dionex CG17 and then separated on a Dionex IonPac CS17 column with 5 mmol·L -1 MSA containing 35% acetonitrile (v / v) , Non-inhibitory conductance detector for detection. Results The method was reproducible. The recoveries ranged from 97.8% to 103.3%. The lowest detection limit was 0.2 μg · mL ~ (-1) and the linearity was good in 0.4 ~ 10 μg · mL ~ (-1). Conclusion The method of on-line matrix elimination-ion chromatography for the determination of trace amounts of cations has been established. It can be widely used in the control of cationic residues in pharmaceuticals.