UPLC-Q-TOF测定化妆品中9种硝基苯类化合物  

Determination of nine nitrobenzene compounds in cosmetics by ultra performance liquid chromatography quadrupole-time-of-flight mass spectrometry

作　　者：张科明 刘雪年 邓鸣 鲁毅翔 许杨彪 Keming Zhang;Xuenian Liu;Ming Deng;Yixiang Lu;Yangbiao Xu(Guangxi Institute for Food and Drug Control,Nanning,Guangxi 530021,China;Pharmaceutical College,Guangxi Medical University,Nanning,Guangxi 530021,China)

机构地区：[1]广西食品药品检验所,广西南宁530021 [2]广西医科大学药学院,广西南宁530021

出　　处：《日用化学工业（中英文）》2024年第6期744-750,共7页China Surfactant Detergent & Cosmetics

基　　金：广西食品药品监督管理局科研计划(桂食药科2018-02(直属))。

摘　　要：建立了超高效液相色谱-四极杆-飞行时间质谱筛查确证化妆品中9种硝基苯类化合物的分析方法。样品经乙酸乙酯提取后,钯碳5%Pd催化氢化,以0.1%(V/V)甲酸水-乙腈为流动相在Poroshell 120 EC-C18(100 mm×4.6 mm,2.7µm)色谱柱上进行梯度洗脱,正离子模式下采用信息依赖性扫描(Auto MS/MS CID)模式采集图谱,以保留时间、一级母离子精确质量数、同位素丰度比、二级子离子精确质量数构建筛查数据库并对检测结果检索,实现化妆品中9种硝基苯类化合物的筛查确证,以分子离子精确质量数提取色谱峰面积定量。结果表明,9种硝基苯类化合物的氢化产物线性关系良好,相关系数(r)大于0.999,方法的检出限为0.01~0.3 mg/kg,定量限为0.04~2.0 mg/kg。膏霜、化妆水、爽身粉、唇膏基质在三个加标水平下的回收率为85.2%~113%,RSD为0.23%~3.61%。该法准确、灵敏、专属性好,适用于化妆品中硝基苯类化合物的筛查和定量分析。An ultra performance liquid chromatography-quadrupole-time-flight mass spectrometric method was developed for the simultaneous screening and determination of 9 nitrobenzene compounds,including nitrobenzene(NB),3,4-dinitrotoluene(3,4-DNT),2,3-dinitrotoluene(2,3-DNT),2,4-dinitrotoluene(2,4-DNT),2,6-dinitrotoluene(2,6-DNT),2,5-dinitrotoluene(2,5-DNT),3,5-dinitrotoluene(3,5-DNT),2-nitrotoluene(2-NT)and 1-chloro-4-nitrobenzene(ChNB)in cosmetics.Samples were extracted with ethyl acetate,and the extracts were further hydrogenated using 5%Pd/C catalyst.The target analytes were separated on a Poroshell 120 EC-C18 chromatographic column(100 mm×4.6 mm,2.7µm).Gradient elution was carried out with 0.1%(V/V)formic acid aqueous solution and acetonitrile as the mobile phases.The eluent from the column was further detected using Q-tof MS with information dependent acquisition(Auto MS/MS)mode for MS data acquisition.A database,containing retention time,precise mass of parent ion,isotope abundance ratio and precise mass of fragment ion,was established for screening and confirming the nitrobenzene compounds.The quantitation analysis was carried out by extracting peak area with precise mass.Under optimal conditions,the analytes show good linear relationship within the range,with the correlation coefficient(r)not less than 0.999.The limits of detection are in the range of 0.01-0.3 mg/kg,and the limits of quantification are in the range of 0.04-2.0 mg/kg.Samples,such as cream,lotion,powder and lip balm,are fortified at three levels.The average spiked recoveries range from 85.2%to 113%,with the relative standard deviations(RSDs)ranging from 0.23%to 3.61%.The optimized method is accurate,sensitive,specific and suitable for the detection and screening of nitrobenzene compounds in cosmetics.

关 键 词：超高效液相色谱 四极杆-飞行时间质谱 硝基苯类化合物 化妆品 

分 类 号：TQ658[化学工程—精细化工]