LC-MS/MS法测定QT脂质体注射液用镀膜胶塞中PFOS和PFOA的迁移
Determination of migration of PFOS and PFOA in the coated stopper of QT liposome injection by LC-MS/MS
分类号:R917
出版年·卷·期(页码):2017,37 (7):1314-1319
DOI:
10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------
目的:建立LC-MS/MS法测定QT脂质体注射液用镀膜胶塞中全氟辛基磺酸(PFOS)和全氟辛酸(PFOA)的迁移。方法:采用Symmetry C18(150 mm×3.0 mm,5μm),以0.01 mol·mL-1乙酸铵-乙腈(55:45)为流动相。采用电喷雾离子源(ESI)、负离子模式检测方式进行定量分析。结果:QT脂质体注射液用镀膜胶塞中PFOS和PFOA在8~200 ng·mL-1范围内线性良好(r分别为0.999 8、0.999 9);最低检测限分别为2.000、2.074 ng·mL-1;平均回收率(n=9)分别为 103.7%、105.9%,RSD分别为7.2%、7.5%;日内精密度RSD分别为2.5%、3.0%,日间精密度RSD分别为2.4%、3.1%;QT脂质体注射液用镀膜胶塞中PFOS和PFOA均未检出。结论:QT脂质体注射液样品中均未有PFOS和PFOA迁移。本方法准确、灵敏,经方法学验证,可用于测定QT脂质体注射液用镀膜胶塞中PFOS和PFOA的迁移。
-----英文摘要:---------------------------------------------------------------------------------------
Objective: To establish a LC-MS/MS method for the determination the migration of PFOS and PFOA in the coated stopper of QT liposome injection. Methods: A Waters symmetry C18 (150 mm×3. 0 mm, 5μm) was applied with the mobile phase of 0. 01 mol·mL-1 ammonium acetate-acetonitrile (55:45). Electrospray ionization(ESI) Source was employed and the analytes were detected under the negative ionization method. Results: The calibration curves of PFOS and PFOA were linear in the range of 8-200 ng·mL-1 (r=0. 999 8, 0. 999 9, respectively); the lowest detection limits were 2. 000, 2. 074 ng·mL-1, respectively; the average recoveries (n=9) were 105. 9% and 103. 7% with RSD of 7. 2% and 7. 5% respectively; RSDs of intra-day were 2. 5%, 3. 0% and inter-day were 2. 4%, 3. 1%, respectively;PFOS and PFOA were not detected in QT liposomes. Conclusion: There were no PFOS and PFOA migration in the QT liposome injection. This method is accurate, sensitive and reproducible, which can be applied to the determination of PFOS and PFOA in the coated stopper of QT liposome injection.
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