LC-MS法检测制药设备隔离器的密闭性

Detection the airtightness of pharmaceutical equipment isolators by LC-MS

建立制药设备隔离器密闭性的高效液相色谱-质谱法检测方法。采用WATERS ACQUITY UPLC?BE色谱柱(4.6 mm×150.0 mm,1.7μm),以0.02 mol/L甲酸铵水溶液(用0.1%氨水调节pH值至8.0)-乙腈为流动相,流速为0.5 mL/min,采用质谱检测器,在ESI-模式下采集数据。结果显示,乳糖在23.422 9~468.458 6 ng/mL范围内线性关系良好,线性相关系数r>0.999,定量限溶液质量浓度为23.422 9 ng/mL(0.05μg/m^(3)),检测限溶液质量浓度为7.026 9 ng/mL(0.01μg/m^(3)),PTFE采样膜回收率均在80%~120%。该方法可以准确、灵敏地检测制药设备隔离器的密闭性程度,为共线生产和共用设施区域防止交叉污染及保障人员健康提供了参考依据。

A high performance liquid chromatography-quadrupole mass spectrometry(LC-MS)method was established for detecting the airtightness of pharmaceutical equipment isolators.A WATERS ACQUITY UPLC®BE(4.6 mm×150.0 mm,1.7μm)column was used to isolate compounds,with isocratic elution using pH 8.0 ammonium formate aqueous solution(0.02 mol/L)and acetonitrile as the mobile phases.The flow rate was set at 0.5 mL/min.Using mass spectrum detector,the data were collected in ionization mode ESI-.The results showed that lactose had good linear relationship in the range of 23.4229-468.4586 ng/mL,with linear correlation coefficient r>0.999.The limit of quantitation was 23.4229 ng/mL(0.05μg/m^(3)),and the limit of detection were 7.0269 ng/mL(0.01μg/m^(3)).The recoveries of PTFE sampling films were 80%-120%.The method can accurately and sensitively test the airtightness of pharmaceutical equipment isolators,which provides a reference basis for preventing cross contamination and controlling personnel health exposure risks in areas of collinear production and shared facilities.