漂浮固化分散液液微萃取/气相色谱法测定化妆水中4种增塑剂

Analysis of Phthalate Esters in Lotion by Dispersive Liquid-Liquid Microextraction Based on Solidification of Floating Organic Droplets Combined with Gas Chromatography

建立了漂浮固化分散液液微萃取(DLLME-SFO)-气相色谱法(GC)同时测定化妆水中4种邻苯二甲酸酯类增塑剂(PAEs)的分析方法,并对萃取剂体积、分散剂种类、分散剂体积、萃取时间、水相pH值、盐浓度等参数进行优化。向样品溶液(化妆水和水的体积比为1∶10,pH 3.0)中快速加入15μL 1-十二醇(萃取剂)和1 300μL乙醇(分散剂),涡旋1 min,4 000 r.min-1离心5 min后,于冰浴中浸泡,待1-十二醇凝固后转移,融化后进行气相色谱分析。结果表明,该方法对4种目标化合物的线性范围为5.0～500.0μg.L-1,检出限为0.001～1.0μg.L-1,回收率为88%～108%,相对标准偏差为1.6%～3.3%。4种目标化合物的富集倍数为800～1 578倍。将该方法与其它测定邻苯二甲酸酯类增塑剂的前处理方法进行对比。该方法操作简单快速、灵敏度高,可满足化妆水中邻苯二甲酸酯类增塑剂的分析要求。

A novel dispersive liquid-liquid microextraction based on solidification of floating organic droplets（DLLME-SFO） combined with gas chromatography（GC） was developed,and validated in the pretreatment and determination of four phthalate esters（PAEs）,including dibutyl phthalate,benzyl butyl phthalate,2-ethylhexyl phthalate,and di-n-octyl phthalate in lotion.The experimental conditions affecting extraction efficiencies for the analytes,such as extraction solvent volume,kind of dispersive solvent,dispersive solvent volume,extraction time,pH value and salt concentration were investigated.In the optimal DLLME-SFO method,the sample solution adjusted to pH 3.0 was prepared as a mixed solution of lotion-pure water（1 ∶ 10）.15 μL 1-dodecanol（extraction solvent） and 1 300 μL ethanol（dispersive solvent） were rapidly injected into the sample solution.After vortexed for 1 min and centrifugated at 4 000 r· min-1 for 5 min,the sample was cooled down in an ice bath till 1-dodecanol became solid and formed a small ball.Then the solidified 1-dodecanol phase was transferred,and directly detected by GC method after it melted.As results,the linear ranges of the target PAEs were in the range of 5.0-500.0 μg· L-1.The detection limits ranged from 0.001 μg· L-1 to 1.0 μg· L-1.The recoveries were in the range of 88%-108%with relative standard deviations of 1.6%-3.3%.The enrichment factors for the target analytes ranged from 800 to 1 578.Compared with the other pretreatment methods for the extraction of PAEs,the developed method was simple,rapid,sensitive and accurate,and could be applied in the analysis of phthalate esters in lotion.