超高效液相色谱-串联质谱法快速测定苯磺酸酯类基因毒性杂质

Determination of Genotoxic Impurities Benzenesulfonate Estersby UPLC-MS/MS

目的建立超高效液相色谱-串联质谱快速测定苯磺酸酯类基因毒性杂质含量的分析方法。样品经乙腈超声提取,离心过膜后直接进样,经Kinetex F5色谱柱分离,以0.1%甲酸-乙腈为流动相,梯度洗脱,多反应监测扫描,正离子模式检测,空白基质标准曲线外标法定量。结果显示,在0.2~1000 ng/mL范围内成线性,相关系数大于0.99,该方法专属性、精密度、耐用性、稳定性均良好。结论经过方法学验证,该方法适用于苯磺酸酯类基因毒性杂质含量的测定。

Objective:A method for the rapid determination of Benzenesulfonate Esters by ultra-liquid chromatography tandem mass spectrometry was established.Methods:The sample was extracted by ultrasound using acetonitrile and centrifuged through membrane.Then,10μL supernatant was directly injected into UPLC-MS/MS for analysis.After separated on a Kinetex F5 columnusing formic acid solution and acetonitrile as a mobile phase,methyl benzenesulfonate and ethyl benzenesulfonate were detected by mass spectrum in the multi-reaction monitoring mode via positive electrospray ionization and quantified by external standard method with blank matrix curve.Results:No interference was observed and the linear range was 0.2~1000 ng/mL with a correlation coefficient(r)of 0.99.Under the chromatographic conditions,benzenesulfonate esters showed good specificity,precision,durability and stability.Conclusion:Our method is suitable for the determination of benzenesulfonate esters through the methodology validation.