微滴液相微萃取技术用于气相色谱-质谱法分析药品中的酞酸酯和对羟基苯甲酸酯

Application of single drop microextraction in the determination of phthalate esters and parabens in drugs by gas chromatography-mass spectrometry

应用微滴液相微萃取(SDME)与气相色谱-离子阱质谱联用测定药品中的酞酸酯和对羟基苯甲酸酯。考察了萃取溶剂的种类及用量、微液滴在样品溶液中的深度、萃取时间及搅拌子的搅拌速度对微滴液相微萃取效果的影响。优化的萃取条件:萃取溶剂为1.5μL甲苯,微液滴在样品溶液中的深度为0.8cm,搅拌子的搅拌速度为1000r/min,萃取时间为20min。该方法的线性范围为0.032~80mg/L,检出限为0.6μg/L^1.28mg/L,加标回收率为95.85%~148.85%,相对标准偏差为3.9%~14.9%。

Single drop microextraction （SDME） was used for the determination of phthalate esters and parabens in drugs by gas chromatography-ion trap mass spectrometry （GC-IT/MS）. The effects of the nature of extraction solvents, microdrop volume, the depth of microdrop in sample solution, extraction time and stirring rate on the extraction efficiency were investigated separately. The optimal SDME conditions, 1.5 μL of toluene, 0.8 cm of the depth of microdrop, 1 000 r/min of stirring rate and 20 min of extraction time, were obtained and used for the analysis of methylparaben （MP）, ethylparaben （EP）, propylparaben （PP）, iso-propylparaben （IPP）, butylparaben （BP）, dimethyl phthalate （DMP）, diethyl phthalate （DEP） and dibutyl phthalate （DBP） in drugs. The results showed that the working curves for 8 phthalate esters and parabens were linear in the range of 0.032-80 mg/L by GC-MS on selective ion storage mode. The limits of detection （LOD） were between 0.6 μg/L and 1.28 mg/L, the overall recoveries were 95.85%-148.85% with the relative standard deviations of 3.9%-14.9%.