正己烷除脂结合QuEChERS-气相色谱-串联质谱法测定化妆品中12种N-亚硝胺类化合物的含量  

Determination of 12 N-Nitrosamines in Cosmetics by Gas Chromatography-Tandem Mass Spectrometry with Combination of n-Hexane Degreasing and QuEChERS

作　　者：李劲松 童文烽 徐巧 王天琦 李剑 严青 LI Jinsong;TONG Wenfeng;XU Qiao;WANG Tianqi;LI Jian;YAN Qing(Hangzhou Puyu Technology Development Co.,Ltd.,Hangzhou 311300,China)

机构地区：[1]杭州谱育科技发展有限公司,杭州311300

出　　处：《理化检验（化学分册）》2024年第11期1141-1147,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：取1 g样品,加入10μg·L^(-1)混合同位素内标溶液、10 m L乙腈、1 m L水和0.5 g氯化钠,匀浆2 min,超声30 min,离心10 min,在上清液中加入2 m L正己烷,振荡5 min,静置分层,在下层相中依次加入200 mg N-丙基乙二胺(PSA)、200 mg C18和1 500 mg无水硫酸镁,振荡5 min,离心10 min。取1 m L上清液,于25℃氮吹至近干,加入1 m L乙酸乙酯复溶,过0.22μm聚四氟乙烯(PTFE)针式过滤头,滤液供气相色谱-串联质谱法分析。在HP-INNOWAX色谱柱上以程序升温条件分离各N-亚硝胺类化合物,以电子轰击离子源电离,多反应监测(MRM)模式检测,同位素内标法定量。结果显示:12种N-亚硝胺类化合物的质量浓度均在一定范围内和对应的响应值与内标响应值的比值呈线性关系,检出限(3S/N)为0.17~0.66μg·kg^(-1)。对5种类型化妆品空白基质进行5,20,100μg·kg^(-1)加标水平的回收试验,回收率为81.6%~117%,测定值的相对标准偏差(n=6)为1.2%~4.8%。方法用于市售5种类型化妆品样品的分析,均未检出12种N-亚硝胺类化合物。The 1 g of sample was taken,and 10μg·L^(−1) mixed isotope internal standard solution,10 mL of acetonitrile,1 mL of water,and 0.5 g of sodium chloride were added.After homogenizing for 2 min,sonicating for 30 min,and centrifuging for 10 min,2 mL of n-hexane was added into the supernatant,and the mixed solution was shaken for 5 min,and settled until the solution was separated into layers.Then 200 mg of N-propylethylenediamine(PSA),200 mg of C18,and 1500 mg of anhydrous magnesium sulfate were added into the lower phase in sequence,and the mixture was shaken for 5 min,and centrifuged for 10 min.The 1 mL of supernatant was taken,and blown to near dryness at 25℃by nitrogen.The residue was re-dissolved by 1 mL of ethyl acetate,and passed through a 0.22μm PTFE needle filter,and the filtrate was analyzed by gas chromatography-tandem mass spectrometry.N-Nitrosamines were separated on HP-INNOVAX chromatographic column under programmed temperature conditions,ionized by electron impact ion source,detected in multiple reaction monitoring(MRM)mode,and quantified by isotope internal standard method.It was shown that linear relationships between the mass concentrations of 12 N-nitrosamines and response value ratios of the targets to internal standards were kept in definite ranges,with detection limits(3S/N)in the range of 0.17-0.66μg·kg−1.Test for recovery was conducted on 5 types of cosmetic blank matrices at spiked levels of 5,20,100μg·kg−1,giving recoveries in the range of 81.6%-117%,and RSDs(n=6)of the determing values in the range of 1.2%-4.8%.The proposed method was used for the analysis of 5 types of cosmetics samples on the market,and 12 N-nitrosamines were not detected.

关 键 词：化妆品 N-亚硝胺类化合物 气相色谱-串联质谱法 QUECHERS 同位素内标法 

分 类 号：O657.63[理学—分析化学]