防晒类化妆品中2种帕地马酯的高效液相色谱检测及质谱确证

Determination of Padimates in Sunscreen Cosmetics by HPLC and Their Verification by LC-MS/MS

建立了同时测定防晒类化妆品中帕地马酯A和帕地马酯O的高效液相色谱分析方法及质谱确证方法。化妆品样品以甲醇为提取溶剂进行超声提取,提取液离心处理,取上清液经微孔滤膜过滤后测定。采用XTerra MS C18柱（250×4.6mm,5μm）分离,外标法定量。结果表明防晒类化妆品中帕地马酯A和帕地马酯O的方法定量限均为0.5mg/kg,在低、中、高3个添加水平范围内平均回收率为89.1%~112.5%,相对标准偏差为2.0%~7.7%。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、快速、灵敏度高,适用于防晒类化妆品的实际检验工作。

A high-performance liquid chromatographic （HPLC） method has been developed for the simultaneous determination of padimate A and padimate O in sunscreen cosmetics. A liquid chromatography-tandem mass spectrometric （LC-MS/MS） method was also established for the verification of the analytical results. Cosmetic samples were ultrasonically extracted with methanol, centrifuged, and filtered by microporous membrane filter. The chromatographic separation of the analytes were performed using an XTerra MS C18 column （250 × 4.6 mm, 5 μm）. The quantitation was carried out by external standard method. The experimental results indicated that the limits of quantitation（LOQs） for padimate A and padiamte O were both 0. 5 mg/kg. The mean recoveries at three spiked levels ranged from 89.1% to 112.5% with the relative standard deviations （RSDs） between 2.0 and 7.7%. The suspected positive samples were subjected to further verification by LC-MS/MS. The method is accurate,rapid, sensitive,and can be used for the testing of sunscreen cosmetics.