摘要
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。
Comprehensive analytical methods have been developed for the simultaneous determination of sixhalogenated salicylanilidesin cosmetics by high performance liquid chromatography（HPLC） and high performance liquid chromatography tandem mass spectrometry（HPLC-MS/MS）. Cosmetic samples were ultrasonically extracted with methanol. The extract was centrifuged,and then filtered througha microporous membrane. The chromatographic separation of the analyteswereperformedusing an Eclipse XDB-Phenyl（4. 6 mm× 250 mm,5 μm） column with isocratic elution. The quantitation was carried out by external standard method.The experimental results indicated that the limits of quantitation（LOQs） for the sixhalogenated salicylanilides were 10 mg/kg. The mean recoveries at three spiked levels ranged from 89. 4% to 107. 8% with the relative standard deviations（RSDs） between 2. 1% and 6. 7%. The suspected positive samples were subjected to further verification by HPLC-MS/MS. The method is accurate,rapid,sensitive,and can be used for the inspection of cosmetics.
出处
《分析试验室》
CAS
CSCD
北大核心
2016年第9期1033-1037,共5页
Chinese Journal of Analysis Laboratory
基金
中华人民共和国工业与信息化部行业标准计划项目(2015-0129T-QB)资助
关键词
化妆品
卤代水杨酰苯胺
高效液相色谱
高效液相色谱-串联质谱
Cosmetics
Halogenated salicylanilides
High performance liquid chromatography（HPLC）
High performance liquid chromatographytandem mass spectrometry（HPLC-MS/MS）
