化妆品原料植物提取物中N-亚硝基二甲胺和N-亚硝基二乙胺含量的测定  

Determination of N-nitrosodimethylamine and N-nitrosodiethylamine in Plant Extracts of Cosmetics raw Materials

作　　者：周卓为 吴梦仰 林剑豪 钟怀香 甘达有 ZHOU Zhuowei;WU Mengyang;LIN Jianhao;ZHONG Huaixiang;GAN Dayou(CAS Testing Technical Services(Guangzhou)Co.,Ltd.,Gangdong Guangzhou 510650,China)

机构地区：[1]中科检测技术服务(广州)股份有限公司,广东广州510650

出　　处：《广州化工》2025年第4期68-70,共3页GuangZhou Chemical Industry

摘　　要：建立了气相色谱-三重四极杆质谱法(GC-MS/MS)测定植物提取物中N-亚硝基二甲胺(NDMA)和N-亚硝基二乙胺(NDEA)含量的方法。样品采用二氯甲烷提取后,氮气浓缩定容,经DB-624(60 m×0.32 mm×1.8μm)色谱柱程序升温分离,在多反应监测(MRM)模式下分析,含量计算为内标法。结果表明, NDMA和NDEA分别在3.4~150μg/L和1.3~40μg/L范围内线性关系良好(r>0.998),检出限分别为0.13和0.06μg/kg,定量限分别为0.34和0.13μg/kg。NDMA在0.34、 4和15μg/kg加标水平下平均回收率为86.07%~106.13%,相对标准偏差为6.79%~8.78%;NDEA在0.13、 1和4μg/kg加标水平下平均回收率为91.80%~117.30%,相对标准偏差为8.77%~11.84%。采用该方法测定市售的艾叶提取物、百合提取物、薄荷提取物各5个批次,均未检出NDMA和NDEA。该方法前处理简单高效,专属性强,灵敏度高,准确性好,可用于化妆品原料植物提取物中NDMA和NDEA的筛查和含量测定。An analytical method was established for the determination of N-nitrosodimethylamine and N-nitrosodiethylamine in plant extracts by gas chromatography-triple quadrupole mass spectrometry.The samples were extracted with dichloromethane,concentrated and diluted with nitrogen,the analytes were separated by gas chromatographic column DB-624(60 m×0.32 mm×1.8μm)following GC temperature program.Mass spectrometric ionization was undertaken in electron impact(EI)ionization mode,and MS detector was operated in multiple reaction monitoring(MRM)mode including quantitative ion pair and qualitative ion pair for all analytes.The results showed that N-nitrosodimethylamine and N-nitrosodiethylamine had good linear relationships in the ranges from 3.4 to 150μg/L and 1.3 to 40μg/L,respectively(r>0.998).The detection limits were 0.13 and 0.06μg/kg,and the quantitative limits were 0.34 and 0.13μg/kg,respectively.The average recoveries of NMDA at the spiked levels of 0.34,4,15μg/kg were from 86.07%to 106.13%,and the relative standard deviations(RSDs)were from 6.79%to 8.78%.The average recoveries of NDEA at 0.13,1,4μg/kg spiked levels were 91.80%to 117.30%,and RSDs were from 8.77%to 11.84%.N-nitrosodimethylamine and N-nitrosodiethylamine were not detected in five batches of commercially available Artemisia argyi extract,lily extract and mint extract by this method.The method had the advantages of simple and efficient pretreatment,strong specificity,high sensitivity and good accuracy.It can be used for screening and content determination of N-nitrosodimethylamine and N-nitrosodiethylamine in plant extracts of cosmetic raw materials.

关 键 词：GC-MS/MS 化妆品原料 植物提取物 NDMA NDEA 

分 类 号：O656.31[理学—分析化学] O657.63[理学—化学]