摘要
建立了气相色谱-质谱(GC-MS)联用技术测定药用丁基橡胶塞中18种多环芳烃(PAHs)。用正己烷-丙酮(体积比1∶1)对样品进行超声极限浸提,浸提液经固相萃取柱净化后,用DB-EUPAH柱(60 m×0.25 mm×0.25μm)分离,质谱以选择离子监测(SIM)模式检测,内标法定量。对浸提溶剂、浸提比例和极限浸提进行考察后,在优化条件下,PAHs的峰面积与质量浓度在低浓度范围1~10 ng/mL和高浓度范围10~200 ng/mL均呈现良好的线性关系,线性相关系数r均大于0.9992。方法检出限(LOD)为0.2~10 ng/g,定量限(LOQ)为1~10 ng/g。在1、10和100 ng/g加标水平下的平均回收率为76.63%~113.93%,相对标准偏差(RSD,n=3)为0.11%~6.86%。该方法灵敏度高、准确性好,适用于药用丁基橡胶塞中18种PAHs含量的同时测定。
A gas chromatography-mass spectrometry(GC-MS)method was established for the determination of 18 polycyclic aromatic hydrocarbons(PAHs)in butyl rubber closures.PAHs in samples were exhaustively extracted by ultrasonic extractor with n-hexane-acetone(1∶1,by volume).The extract was purified by solid phase extraction column and analyzed by GC-MS with selected ion monitoring model.Internal standard method was adopted for PAHs’quantification.The extraction solvent,extraction ratio and exhaustive extraction were investigated.Under the optimized experimental conditions,the calibration curves of PAHs showed good linearities both in the range of 1-10 ng/mL and 10-200 ng/mL with correlation coefficients larger than 0.9992.The limits of detection were in the ranges of 0.2-10 ng/g,while the limits of quantitation varied from 1 ng/g to 10 ng/g.The average recoveries at three spiked levels of 1,10 and 100 ng/g were in the range of 76.63%-113.93%with the relative standard deviations(n=3)of 0.11%-6.86%.This method is suitable for the simultaneous determination of 18 PAHs in pharmaceutical butyl rubber closures with high sensitivity and accuracy.
作者
薄晓文
张敏
郭利娟
刘雪婷
沈永
BO Xiaowen;ZHANG Min;GUO Lijuan;LIU Xueting;SHEN Yong(Shandong Institute of Medical Device and Pharmaceutical Packaging Inspection,Jinan250101;NMPA Key Laboratory for Quality Control of Pharmaceutical Packaging,Jinan250101;Shandong Key Laboratory of Biological Evaluation for Medical Devices,Jinan250101)
出处
《分析科学学报》
CAS
CSCD
北大核心
2021年第5期680-685,共6页
Journal of Analytical Science
基金
山东省医疗器械产品质量检验中心科研资助项目(No.ZX202005)。
关键词
药用丁基橡胶塞
多环芳烃
极限浸提
气相色谱-质谱联用法
Pharmaceutical butyl rubber closure
Polycyclic aromatic hydrocarbons
Exhaustive extraction
GC-MS
