UPLC-Q-TOF-MS法测定化妆品和消毒产品中108种非法添加化合物

Determination of 108 illegally added compounds in cosmetics and disinfectants by UPLC-Q-TOF-MS

建立了超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF-MS)进行筛查和确证化妆品和消毒产品中108种非法添加化合物的方法。样品采用饱和氯化钠溶液涡旋分散后,加入含0.05%(体积分数)甲酸的乙腈溶液超声提取,冷冻离心,X-Bridge C_(18)色谱柱(4.6 mm×100 mm,3.5μm)分离。在电喷雾离子源、正负离子扫描模式下,通过宽谱碰撞诱导解离(bbCID)模式采集待测物的质谱信息,构建108种非法添加化合物的筛查数据库。实验比较了提取溶剂的影响,优化了色谱条件和质谱条件,考察了凝胶剂、膏霜剂和粉剂的基质效应和回收率。结果表明,108种化合物的检出限为0.05~2.25 mg/kg,定量限为0.15~7.50 mg/kg,线性关系良好,相关系数(R^(2))均不低于0.99,3个浓度水平的加标回收率为60.0%~122.1%、相对标准偏差(RSD)为1.2%~23.3%。应用该方法对83份化妆品和50份消字号抑菌制剂进行分析,最终从两份消毒产品中确证检出林可霉素和利多卡因,其含量分别为5024.4和2.2 mg/kg。该方法操作简便,准确性好,适用于化妆品和消毒产品中多类非法添加化合物的筛查确证和定量分析,具有较强的应用价值。

An ultra-performance liquid chromatography-quadrupole-time of flight mass spectrometry method(UPLCQ-TOF-MS)was established to identify 108 illegally added compounds in cosmetic and disinfectants.Samples were dispersed in a saturated sodium chloride solution,extracted by sonication with acetonitrile solution containing 0.05%formic acid,and frozen at 0℃while centrifuged.Chromatographic separation was performed on a X-Bridge C_(18) column(4.6 mm×100 mm,3.5μm)with gradient elution using 0.1%(volume fraction)acetic acid aqueous solution and acetonitrile as the mobile phases.The mass spectrum information of the tested compounds was collected by broadband collision-induced dissociation(bbCID)mode under the electrospray ion source and positive and negative ion scanning mode,and a screening database of 108 illegally added compounds was constructed.The effect of extraction solvent was investigated and the chromatographic and mass spectrometry conditions were optimized.The matrix effects and recovery of gel-,cream-,and powder-based cosmetics were also investigated.The results show that the detection limit of 108 compounds is 0.05-2.25 mg/kg,and the limit of quantification is 0.15-7.50 mg/kg.The correlation coefficient(R^(2))are greater than 0.99 in the corresponding liner concentration range.Average recoveries are in the range of 60.0%-122.1%at three spiked levels,and the relative standard deviations(RSDs)are 1.2%-23.3%.A total of 83 cosmetics and 50 antibacteriostatic samples are analyzed by this established method.Finally,lincomycin and lidocaine are detected in two batches of disinfection products.The contents of lincomycin and lidocaine are 5024.4 mg/kg and 2.2 mg/kg,respectively.The optimized method is simple,accurate and suitable for rapid screening and simultaneous quantitative analysis of various illegally added compounds in cosmetics and disinfectants.