HF-LPME-GC测定PVC输液管路中6种邻苯二甲酸酯的迁移

目的: 将中空纤维膜液相微萃取(HF-LPME)与气相色谱技术相结合,建立PVC输液管路中6种邻苯二甲酸酯迁移量的测定方法.方法: 通过优化影响萃取富集效率的实验条件,选择长度为1.5 cm的聚丙烯中空纤维膜,以含有苯甲酸苄酯(内标)的甲苯为萃取溶剂,在500 r·min^-1搅拌下,萃取30 min,取萃取液1.0 μL直接进样,进行气相色谱分析.采用DB-5MS石英毛细管柱(30 m×0.25 mm×0.25 μm),程序升温,进样口温度250 ℃;FID检测器温度300 ℃,载气为氮气.结果: 该方法对6种邻苯二甲酸酯的富集倍数在151~1189倍之间.检测限(S/N=3)为0.2~7.5 μg·L^-1,加标回收率为85.6%~98.5%,RSD为4.0%~11.0%.结论: 本方法灵敏、简便,适用于PVC输液管路邻苯二甲酸酯迁移量的检测.

Objective: To develop a method for simultaneous determination of six kinds of phthalate esters released from PVC medical tube by hollow fiber-based liquid phase microextraction (HF-LPME) coupled with gas chromatography. Methods: After optimizing the main experimental parameters which might influence extraction enrichment efficiency, polypropylene hollow fiber membrane with length of 1.5 cm was selected as the carrier, and toluene containing benzyl benzoate (internal standard) was selected as the extraction and impregnation solvent.The extraction was carried out at a stirring rate of 500 r·min^-1 for 30 min, then 1.0 μL of extraction solvent was directly injected into GC for analysis. The separation was performed on the DB-5MS capillary column (30 m×0.25 mm×0.25 μm) with nitrogen as the carrier gas, the oven temperature was raised by programming, the injector temperature was 250 ℃, and the FID detector temperature was set at 300 ℃. Results: The method exhibited enrichment factor values ranging from 151 to 1189. The limits of detection (LOD) ranged from 0.2 μg·L^-1to 7.5 μg·L^-1(S/N=3).The recoveries ranged from 85.6% to 98.5% with relative standard deviations (RSDs) between 4.0% to 11.0%. Conclusion: The method is sensitive, simple and suitable for determination of phthalate esters released from medical PVC tube.

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