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建立了同时测定化妆品中6种卤代水杨酰苯胺的高效液相色谱检测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进行高效液相色谱测定。采用Eclipse XDBPhenyl(4.6 mm×250 mm,5μm)色谱柱进行分离,等度洗脱,外标法定量。化妆品中6种卤代水杨酰苯胺的方法定量限为10 mg/kg,在低、中、高3个添加水平范围内平均回收率在89.4%~107.8%之间,相对标准偏差为2.1%~6.7%。对于疑似阳性样品,进一步采用高效液相色谱-串联质谱法进行确证分析。方法适用于化妆品的实际检测。
A method for the simultaneous determination of six halofluoro salicylanilides in cosmetics by high performance liquid chromatography and mass spectrometry was established. Cosmetic samples were extracted with methanol as the ultrasonic extraction, the extract was centrifuged, the supernatant was filtered through a microporous membrane and then subjected to high performance liquid chromatography. Using Eclipse XDBPhenyl (4.6 mm × 250 mm, 5μm) column separation, isocratic elution, external standard quantitative. The limits of quantification of 6 halonsalicyanilides in cosmetics were 10 mg / kg. The average recoveries were 89.4% -107.8% at low, medium and high levels with the relative standard deviation of 2.1% ~ 6.7%. For suspected positive samples, confirmatory analysis was further performed using high performance liquid chromatography-tandem mass spectrometry. The method is suitable for the actual testing of cosmetics.