化妆品中10种邻苯二甲酸酯的HPLC联合GC-MS测定法  

Determination of ten phthalate esters (PAEs) in cosmetics by HPLC combined with GC-MS

作　　者：刘菁[1] 米亚娴[1] 李华龙[1] 

机构地区：[1]天津市药品检验所,300070

出　　处：《职业与健康》2015年第20期2765-2768,共4页Occupation and Health

摘　　要：目的建立一种高效、准确、灵敏的化妆品中10种邻苯二甲酸酯的高效液相色谱（HPLC）测定方法,并用气相色谱-质谱（GC-MS）法对阳性结果进行进一步确证。方法用甲醇提取化妆品中的邻苯二甲酸酯,经VP-ODS（250 mm×4.6 mm,5μm）柱分离,以甲醇-乙腈-水为流动相以梯度洗脱的方式进行色谱分离,以二极管阵列检测器进行检测及初步定性鉴别,于280 nm处进行定量测定。样品中的阳性结果用气GC-MC法进行进一步确证。结果 10种邻苯二甲酸酯均达到基线分离,并在0~0.8 mg/ml浓度范围内与峰面积呈良好的线性关系;低、中、高3个水平回收率分别为95.0%~108.2%、97.0%~102.5%、95.6%~104.6%;最低检出限在0.5~3 ng之间。结论该方法简便、灵敏、专属性好,可同时测定化妆品中10种邻苯二甲酸酯类化合物的量。GC-MC法的应用对阳性样品的确认提供了保证。[Objective]To establish an efficient,accurate and sensitive method for the determination of ten phthalate esters（PAEs）in cosmetics by HPLC, confirm the positive results by GC-MS. [Methods]The samples were extracted by methanol and qualitatively determined by HPLC with PDA detector. The separation of 10 PAEs was carried out on VP-ODS（250 mm×4.6 mm,5 μm） column by gradient elution of concentration with mobile phase consisting of methanol,acetonitrile and water. The quantification of 10 PAEs was based on detection wavelength at 280 nm. The positive results of the samples were further confirmed by GC-MS. [Results]A good separation for 10 PAEs was achieved. The linear ranges of the calibration curves for10 PAEs were between 0 mg/ml and 0.8 mg/ml. The average recoveries at low,middle and high levels of 10 PAEs were 95.0%-108.2%,97.0%-102.5% and 95.6%-104.6% respectively. The limits of detection（LODs） for 10 PAEs were in the range from 0.5 ng to 3 ng. [Conclusion]The method is simple and sensitive with good specificity,which can meet the needs of simultaneous determination of 10 PAEs in cosmetics. GC-MS provides the guarantee for the confirmation of the positive samples.

关 键 词：化妆品 邻苯二甲酸酯 HPLC GC-MS 

分 类 号：R115[医药卫生—公共卫生与预防医学]