文献类型：期刊文献

中文题名：LC-MS级乙腈溶剂适应性检测方法

英文题名：Suitability Test for LC-MS Grade Acetonitrile Solvent

作者：凌芳[1];郑琦[1];倪传宏[1];洪亚云[2];赵红莉[2];徐洁[2]

机构：[1]国药集团化学试剂有限公司,上海200002;[2]华东理工大学分析测试中心,上海200237

年份：2015

卷号：37

期号：4

起止页码：339

中文期刊名：化学试剂

外文期刊名：Chemical Reagents

收录：CSTPCD;;北大核心:【北大核心2014】；

基金：上海市科委"科技创新行动计划"化学试剂研究项目(13142201000)

语种：中文

中文关键词：ESI+;ESI-;标准物;LC-MS级乙腈;适应性检测

外文关键词：ESI＋ ; ESI - ; standard substances ; LC-MS grade acetonitrile solvent ; LC-MS suitability detection

摘要：旨在建立液质联用(LC-MS)级乙腈溶剂适应性检测方法。将利血平、咖啡因作为LC-MS试剂的电喷雾电离源正离子模式(ESI+)指标的标准物,4-硝基苯酚作为LC-MS试剂的负离子模式(ESI-)指标的标准物,在待测乙腈中加入定量的标准物质,在相应的电离模式下,采用质谱仪直接进样。通过改变样品电压、进样速度、N2流速及脱溶剂气温度等条件来选取最佳实验条件,并在最佳实验条件下对配制好的进口和国产待测LC-MS级乙腈标准物溶液分别进行检测,对比两者质谱图的信号强度以及杂峰数量来判断纯度的差异。检测结果表明,所建立方法适用于LC-MS级乙腈溶剂的适宜性检测。此外,国产待测LC-MS级乙腈试剂的纯度基本与进口LC-MS级乙腈相同,能够达到检测要求。
This work aimed to establish a suitability detection method for LC-MS grade acetonitrile solvent. As the standard sub- stances,reserpine and caffeine were chosen for electrospray positive ionization （ ESI＋ ） indicators and p-nitrophenol was for elec- trospray negative ionization （ ESI- ） indicators. Quantitative standard substances were added to the undetermined LC-MS acetoni- trile which was directly detected by mass spectrometry under the corresponding ionization mode. Experimental parameters such as sample voltage,injection rate, N2 flow rate and desolvation temperature were optimized. Under the optimized conditions, the impor- ted and domestic LC-MS acetonitrile which contained quantitative standard substances were further detected. By comparing the signal strength and the number of impurity peaks in two spectra, the purity of the two reagents was determined. The established method can be applied to the suitability detection of LC-MS grade acetonitrile solvent. Besides,the purity of the domestic acetoni- trile reagent is essentially the same as that of the import acetonitrile reagent,which can meet the needs of detection.