化妆品中邻苯二甲酸二异已酯的高效液相色谱检测及质谱确证  

Determination of Diisohexyl phthalate in cosmetics by HPLC and their verification by HPLC-MS/MS

作　　者：郭项雨[1] 陈云霞[1] 李文雅[1] 夏德富 白桦[1] 马强[1] GUO Xiangyu;CHEN Yunxia;LI Wenya;XIA Defu;BAI Hua;MA Qiang(Chinese Academy of Inspection and Quarantine,Beijing,100176,China)

机构地区：[1]中国检验检疫科学研究院,北京100176

出　　处：《质量安全与检验检测》2023年第4期76-79,共4页QUALITY SAFETY INSPECTION AND TESTING

基　　金：国家市场监督管理总局科技计划项目(2022MK192);中央级公益性科研院所基本科研业务费专项资金项目(2022JK17)。

摘　　要：本研究建立了化妆品中邻苯二甲酸二异已酯的高效液相色谱分析及质谱确证方法。膏霜和乳液类样品经氯化钠破乳后用甲醇进行超声辅助溶剂萃取,液体类样品直接用甲醇进行超声辅助溶剂萃取,提取液离心处理,取上清液经微孔滤膜过滤后上机测定。采用Innoval C_(18)(4.6 mm×250 mm,5μm)色谱柱进行分离,以乙腈∶水=90∶10(体积比)为流动相进行等度洗脱,外标法定量。化妆品中邻苯二甲酸二异已酯的方法检出限为2 mg/kg,定量限为5 mg/kg,在5~500 mg/kg线性范围内,呈现良好线性关系(r>0.999)。在低、中、高3个添加水平范围内平均回收率在86.7%~107.6%之间,相对标准偏差为2.9%~6.9%。对于疑似阳性样品,进一步采用液相色谱-串联质谱法进行确证分析。该方法准确、稳定,适用于化妆品中邻苯二甲酸二异已酯的分析测定。A high-performance liquid chromatographic(HPLC)method has been developed for the determination of diisohexyl phthalate in cosmetics.A liquid chromatography-tandem mass spectrometric(LC-MS/MS)method was also established for the verification of the analytical results.Cream and emulsion samples were subjected to sodium chloride demulsification and solvent-ultrasound-assisted extraction with methanol,while water samples were directly subjected to solvent ultrasound-assisted extraction with methanol.And then,the cosmetic samples were centrifuged,and filtered by microporous membrane filter.The chromatographic separation of the analytes were performed using an Innoval C_(18)(4.6 mm×250 mm,5μm)column.Acetonitrile and water(volume ratio 90:10)was used as mobile phase for equal degree elution,and the quantitation was carried out by external standard method.The experimental results indicated that the limits of detection(LOD)and quantitation(LOQ)were 2 and 5 mg/kg,respectively.Satisfactory linearity for analyte was obtained,with correlation coefficients greater than 0.999.The mean recoveries at three spiked levels ranged from 86.7%-107.6%with the relative standard deviations(RSDs)between 2.9%-6.9%.The suspected positive samples were subjected to further verification by LC-MS/MS.The method is accurate,stable,and suitable for the determination of diisohexyl phthalate in cosmetics.

关 键 词：高效液相色谱法 邻苯二甲酸二异已酯 化妆品 塑化剂 

分 类 号：O657.72[理学—分析化学]