固相萃取-超高效液相色谱-串联质谱法测定祛痘化妆品中4种林可胺类化合物  

Simultaneous Determination of Four Lincosamides in Acne Cosmetics by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：卢剑[1] 武中平[1] 车文军[1] 洪华[1] 冼燕萍 郭新东 

机构地区：[1]江苏省产品质量监督检验研究院/国家化妆品质量监督检验中心,江苏南京210007 [2]广州质量监督检测研究院,广东广州510110

出　　处：《香料香精化妆品》2015年第3期33-37,共5页Flavour Fragrance Cosmetics

摘　　要：采用固相萃取净化技术和超高效液相色谱-串联质谱方法（UPLC-MS/MS）,建立了测定祛痘化妆品中4种林可胺类化合物（林可霉素、克林霉素、克林霉素磷酸酯和吡利霉素）的分析方法。样品用酸化乙腈提取,阳离子交换固相萃取小柱（MCX）净化,以乙腈-10mmoL/L乙酸铵溶液（pH 3.0）为流动相,经C18色谱柱梯度洗脱分离,电喷雾正离子模式电离,多反应监测模式检测,外标法定量。结果表明,4种林可胺类化合物的方法定量限（LOQs）均为10μg/kg;在5～200μg/L范围内线性关系良好,相关系数均大于0.999 0;在祛痘膏、祛痘水样品中进行10、100、1 000μg/kg 3个添加水平试验,平均回收率范围为87%～105%,相对标准偏差（n=6）在3.3%～10.2%之间。采用此方法测定了祛痘化妆品中林可胺类化合物的含量水平,发现存在违规添加现象。An analytical method for the determination of 4 lineosamides（lineomycin, clindamyein, clindamycin phosphate and pirlimycin） in acne cosmetics was developed using ultra performance liquid chromatography with tandem mass spectrometry （UPLC-MS/MS） and solid phase extraction （SPE） clean-up. The homogenized sample was extracted with acidified acetonitrile. Sample concentration and purification were performed on a MCX solid extraction cartridge. The separation of 4 lincosamides were subsequently carried out on a C18 column with acetonitrile and 10 mmoL/L armnaonium acetate solution （pH 3. 0） by gradient elution. The analytes were detected by the multiple reaction monitoring （MRM） mode. Identification was based on the retention time and ion ratio, quantification was carried out with the external standard curves. Under the optimal conditions, the quantitation limit of the method for 4 compounds were 10μg/kg. The linear ranges were from 5μg/L to 200μg/L for lincosamides and the correlation coefficients were all greater than 0. 999 0. The average recoveries for acne cream and acne water samples at three spiked concentrations of 10, 100 and 1 000μg/kg were in the range of 87% to 105% with relative standard deviations （RSDs, n = 6） between 3. 3% and 10, 2%. The level of lincosamides in acne cosmetics were determined by using this method, iincomycin and clindamycin were found in some samples.

关 键 词：祛痘化妆品 固相萃取 超高效液相色谱-串联质谱法 林可胺类化合物 

分 类 号：TQ658[化学工程—精细化工] O657.63[理学—分析化学]