气相色谱-串联质谱法同时测定染整助剂中乙二醇醚及其醋酸酯残留量

以乙酸乙酯为萃取溶剂对染整助剂中残留的乙二醇醚及其醋酸酯进行超声萃取后,经WatersSep-PakVacSilica(1g/6mL)固相萃取柱净化,选用DB-Wax色谱柱(60m×0.25mm×0.25μm)分离,采用气相色谱-串联质谱(GC-MS/MS)方法进行多反应监测(MRM)分析,外标法定量,建立了同时测定染整助剂中15种乙二醇醚和4种乙二醇醚醋酸酯的分析方法。结果显示,19种待测物峰面积(A)与其质量浓度(ρ)在一定范围内呈线性相关,相关系数均不低于0.9992。分别以3倍信噪比(S/N=3)和S/N=10计算方法检出限(LOD)和定量下限(LOQ),得MOPA和DEGME的LOD均为30μg/kg,DEGDEE的LOD为20μg/kg,EGEE和EGME的LOD均为10μg/kg,其余14种目标分析物的LOD为1~5μg/kg;MOPA和DEGME的LOQ均为100μg/kg,EGEE、EGME和DEGDEE的LOQ分别为20、30、50μg/kg,其余14种目标分析物的LOQ为1~15μg/kg。在低、中、高3个加标浓度水平下的平均加标回收率为82.4%~94.6%,相对标准偏差为2.7%~9.2%。该方法操作简单、灵敏度高、定量下限低,完全满足染整助剂中乙二醇醚及其醋酸酯残留量检测工作的需要。

Simultaneous Determination of Residual Glycol Ethers and Their Acetates in Dyeing and Finishing Additives by Gas Chromatography-Tandem Mass Spectrometry

An effective method was established for the simultaneous determination of fifteen glycol ethers and four glycol ether acetates residues in dyeing and finishing additives by gas chromatography-tandem mass spectrometry(GC-MS/MS).Residual glycol ethers and their acetates in dyeing and finishing additives were ultrasonically extracted with ethyl acetate as extraction solvent.The extract was then purified using a Waters Sep-Pak Vac Silica(1 g/6 mL)solid-phase extraction(SPE)column.The chromatographic separation of 19 target compounds was performed on a DB-Wax(60 m×0.25 mm×0.25μm)column.GC-MS/MS analysis was carried out in multiple reaction monitoring(MRM)mode,and the concentrations of glycol ethers and their acetates were calibrated by the external standard method.The peak areas(A)for the analytes were linearly related to their mass concentrations(ρ)in each linear range,and the correlation coefficients were no less than 0.999 2.The limits of detection(LODs)and quantitation(LOQs)of the method were calculated by the signal to noise(S/N)ratios of three and ten,respectively.LODs for MOPA and DEGME were both 30μg/kg,LOD for DEGDEE was 20μg/kg,LODs for EGEE and EGME were 10μg/kg,and LODs for the other fourteen target compounds ranged from 1μg/kg to 5μg/kg,while LOQs for EGEE,EGME and DEGDEE were 20,30 and 50μg/kg,respectively,while that for MOPA and DEGME were both 100μg/kg,and LOQs for the other fourteen varied from 1μg/kg to 15μg/kg.The average recoveries at three spiked levels ranged from 82.4%to 94.6%with the relative standard deviations(RSDs)of 2.7%to 9.2%.The proposed method was simple and sensitive,and could meet completely the demands for routine analysis of residual glycol ethers and their acetates in dyeing and finishing additives.