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Determination of phthalate esters in cosmetics by gas chromatography with flame ionization detection and mass spectrometric detection

机译:气相色谱-火焰电离检测和质谱检测气相色谱法测定化妆品中的邻苯二甲酸酯

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摘要

A gas chromatography coupled with flame ionization detection (GC-FID) and mass spectrometric detection (MSD) method was developed to determine the six kinds of phthalate esters [dimethyl phthalate (DMP),diethyl phthalate (DEP),di-n-bu-tyl phthalate (DBP),benzyl butyl phthalate (BBP),di(2-ethylhexyl) phthalate (DEHP) and di-n-octyl phthalate (DOP)] in cosmetics (solid,cream and liquid cosmetics).The cosmetics were extracted with methanol by ultrasonic and then separated with high-speed centrifugation.The upper clear layer was dried and filtered through a 0.45 mum pore diameter filter.The filtrate was injected into GC-FID/GC-MS for detection.GC-FID chromato-gram was applied for qualitative analysis,external standard method was used for quantitative analysis.Confirmation of phthalate presence was undertaken by GC-EI-MS.The recovery range of all phthalates were between 92.0 and 110.0% with relative standard deviations between 1.95 and 5.92%.The low detection limits of the method were:0.1 ng for DMP,DEP,DBP and BBP,0.5 ng for DEHP and DOP.The method had advantages of high precision and sensitivity,simplicity of pretreatment.The method can be used to test the six kinds of phthalate esters in cosmetics.
机译:建立了一种结合火焰电离检测(GC-FID)和质谱检测(MSD)方法的气相色谱法,用于测定六种邻苯二甲酸酯[邻苯二甲酸二甲酯(DMP),邻苯二甲酸二乙酯(DEP),二正丁基]化妆品(固体,奶油和液体化妆品)中的邻苯二甲酸叔丁酯(DBP),邻苯二甲酸苄基丁酯(BBP),邻苯二甲酸二(2-乙基己基)邻苯二甲酸酯(DEHP)和邻苯二甲酸二正辛酯(DOP)。超声分离甲醇,然后进行高速离心分离。将上层透明层干燥并通过0.45微米孔径的过滤器过滤,将滤液注入GC-FID / GC-MS中进行检测.GC-FID色谱图适用于定性分析,采用外标法进行定量分析,采用GC-EI-MS进行邻苯二甲酸盐的确证,所有邻苯二甲酸盐的回收率在92.0%至110.0%之间,相对标准偏差在1.95%至5.92%之间。该方法的低检测限为:0.1 n DMP,DEP,DBP和BBP的克数为0.5,DEHP和DOP的克数为0.5 ng。该方法具有高精度,高灵敏度,预处理简单的优点。该方法可用于测试化妆品中的六种邻苯二甲酸酯。

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