分散相液相微萃取法测定通过输液管后注射液中的邻苯二甲酸酯增塑剂含量

Determination of Phthalate Ester Plasticizers in Injections Passed Through Infustion Set by Dispersive Liquid–liquid Microextraction

关键词:  邻苯二甲酸酯  分散相液相微萃取  气相色谱-质谱联用

Key words:  phthalate esters  dispersive liquid–liquid microextraction  GC-MS

摘要:

目的 采用分散相液相微萃取与GC-MS结合，建立测定通过输液管后注射液中6种邻苯二甲酸酯含量的方法。方法 将30 μL苯甲酸苄酯(内标)的甲苯溶液和20 μL十六烷基三甲基溴化铵溶液快速注入到5.0 mL样品溶液中，旋涡振荡1 min，4 000 r·min^-1离心5 min。弃去水相，使有机相聚集于离心管底部，取1.0 μL萃取液进行CG-MS分析。结果 6种邻苯二甲酸酯的富集倍数为174~280，检测限为(S/N=3)0.007~0.04 ng·mL^-1，加样回收率为97.8%~101.2%，RSD为0.44%~0.93%。在某些通过输液管的注射液中检出DBP和DEHP。结论 本方法灵敏、简便、快速，适用于通过输液管后注射液中微量邻苯二甲酸酯的检测。

Abstract:

OBJECTIVE To develop a method for simultaneous determination of 6 kinds of phthalate esters in injections passed through infustion set by dispersive liquid-liquid microextraction-GC-MS. METHODS A mixture of extraction solvent (toluene containing benzyl benzoate as internal standard) and surfactant (hexadecylytrimethylamminium bromide) solution was injected into 5.0 mL of sample solution to form an emulsion by the assistance of 1 min vortex agitation. After extraction and phase separation by centrifugation under 4 000 r·min^-1 for 5 min, the toluene extract were collected and analyzed by GC-MS. RESULTS The method exhibited enrichment factor values of 6 kinds of phthalate esters ranging from 174 to 280, the 1imits of detection(LOD) ranged from 0.007 to 0.04 ng·mL^-1 (S/N=3). The recoveries were from 97.8% to 101.2% with relative standard deviations (RSD) of 0.44%-0.93%. DBP and DEHP were detected in some injections passed through infustion set. CONCLUSION The method is sensitive, simple and can be applied for simultaneous determination of 6 phthalate esters in injections.