基于纳升电喷雾-便携式离子阱质谱的苯扎氯铵快检方法  

Fast detection of benzalkonium chloride in eye drops based on nano electrospray-portable ion trap mass spectrometry

作　　者：查越 沈学静[1,2] 李明 ZHA Yue;SHEN Xuejing;LI Ming(Central Iron and Steel Research Institute,Beijing 100081;NCS Testing Technology Co.,Ltd.,Beijing 100081)

机构地区：[1]钢铁研究总院,北京100081 [2]钢研纳克检测技术股份有限公司,北京100081

出　　处：《分析试验室》2021年第10期1166-1170,共5页Chinese Journal of Analysis Laboratory

基　　金：国家重点研发计划重大科学仪器设备开发专项(2018YFF0109500)资助。

摘　　要：采用纳升电喷雾源(Nano-ESI)-便携式离子阱质谱(Portable Ion Trap MS)建立了滴眼液杀菌成分苯扎氯铵(BAC)的快速检测方法。在正离子模式下,将滴眼液样品稀释后注入纳升电喷雾源的毛细管,毛细管出口与离子阱质谱进样口距离为10 mm、喷雾电压为2000 V;毛细管电压,毛细管温度和离子漏斗电压分别设为5 V,30℃和40 V。用3种苯扎氯铵的[M-Cl]+峰作为定性判据;用纯物质配制溶液制作定量分析校准曲线。3种苯扎氯铵校准曲线的线性范围1~500 mg/L,相关性系数(R2> 0.99);用11次空白样品测试结果评估方法检出限和定量限为0.1,0.33 mg/L,满足限量判定要求。4种实际样品中3类BAC的定量测定结果同高效液相色谱-质谱法无显著性差异。该方法无需联用色谱,分析时间仅为2 min,可应用于滴眼液等保健品中添加剂苯扎氯铵的快速筛查。In this work,a rapid detection method without using chromatography for the determination of bactericidal component of benzalkonium chloride in commercial eye drops was established by building a nanoelectrospray ionization( Nano-ESI) with portable ion trap mass spectrometer( Ion Trap MS). In the positive ion mode,the eye drops sample was diluted and injected into the capillary for rapid qualitative and quantitative analysis. The optimal analysis conditions were obtained as follows,the distance between the capillary outlet and the injection port was 10 mm,and the spray voltage was 2000 V,the capillary voltage,capillary temperature and ion funnel voltage were set at 5 V,30℃ and 40 V,respectively. The [M-Cl]+peaks of three benzalkonium chlorides were used as qualitative criteria,and the solution was prepared with pure substance and then analyzed by quantitative analysis of standard curves. Under the optimized conditions,the linear range of the three components in the diluted eye drops was 1-500 mg/L with good correlation coefficient( R2> 0. 99). The limit of detection( LOD) of the method evaluated by 11 blank sample test results was 0. 1 mg/L and the limit of quantification( LQD) was 0. 33 mg/L. Compared with the ultrahigh performance liquid chromatography( UPLC)-MS method,there was no significant difference between the quantitative determination results for the actual samples,but the analysis time of the Nano-ESI MS method was shorter( 2 min). Therefore,the method can be used for rapid screening and quantitative determination of benzalkonium chloride as an additive in eye drops.

关 键 词：纳升电喷雾 便携离子阱质谱 苯扎氯铵 快速筛查 

分 类 号：O657.63[理学—分析化学]