摘要
建立了分散液液微萃取(DLLME)结合超高效液相色谱-四极杆/静电场轨道阱质谱(UPLC-Q Exactive Orbitrap MS)同时测定化妆水中抗生素、激素、禁用染料、农药以及真菌毒素5大类共139种药物残留的分析方法。考察了DLLME各条件对萃取效果的影响,确定最佳萃取条件为:取样量5.0 g,萃取剂为四氯乙烷(50μL)、分散剂为乙腈(300μL)、氯化钠用量为0.30 g、超声时间为8 min。样品经萃取后,采用岛津Shimpack XR-ODS II(150 mm×2.0 mm,2.2μm)色谱柱分离,通过Q-Exactive Orbitrap MS以全扫描确定母离子精确质量数的离子丰度,实现多种类目标物的定量,结合保留时间和子离子数据依赖模式扫描(DD-MS2)确定子离子的精确质量数,并配合谱库检索进行快速确证与筛查。结果表明:139种化合物的质量浓度在10~1000 ng/mL范围内与峰强度呈良好线性关系(r>0.99),检出限为10~30μg/kg,回收率为63.0%~95.9%,相对标准偏差(RSD)为3.0%~9.5%;各精确质量数偏差小于3×10^(-6)。该方法稳定、简单、快速、精确,有机试剂用量少,环境友好,适用于化妆水的快速筛查。
An ultra performance liquid chromatography-quadrupole/exactive orbitrap mass spectrometry(UPLC-Q Exactive Orbitrap MS)with dispersive liquid-liquid microextraction(DLLME)was established for the simultaneous determination of 139 drug residues in 5 categories,including antibiotics,hormones,prohibited dyes,pesticides and mycotoxins.The influences of various conditions on the extraction effect of DLLME were investigated.The optimal extraction conditions were as follows:5.0 g of sampling volume,50μL of extraction agent tetrachloroethane,300μL of dispersant acetonitrile,0.30 g of sodium chloride and 8 min of ultrasonic time.After extraction,the samples were separated on a Shimadzu Shim-pack XR-ODS II(150 mm×2.0 mm,2.2μm)column.By using QExactive Orbitrap MS to determine the intensity of the exact mass number of precursor ion in full scan,quantitation on multi-type targets could be realized.Combined with retention time and data-dependent MS/MS(DD-MS2)scanning,the precise mass numbers of the fragment ions could be determined,followed by rapid confirmation and screening with MS/MS spectral library.The results showed that there were good linear relationships for the peak intensities of 139 compounds in mass concentration ranges of 10-1000 ng/mL(r>0.99).The detection limits were 10-30μg/kg,and the recoveries were 63.0%-95.9%,with relative standard deviations(RSDs)between 3.0%and 9.5%.The deviations for each accurate mass number were less than 3×10^(-6).This method is stable,simple,rapid,accurate,low consumption of organic reagents and environmentally friendly,and it is suitable for rapid screening of lotion.
作者
容裕棠
张宪臣
邓晓莹
吴洁珊
刘琼瑜
蔡杰
瓮福良
RONG Yu-tang;ZHANG Xian-chen;DENG Xiao-ying;WU Jie-shan;LIU Qiong-yu;CAI Jie;WENG Fu-liang(Technology Center of Gongbei Customs,Zhuhai 519000,China;Technology Center of Zhongshan Customs,Zhongshan 528403,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2023年第3期264-274,共11页
Journal of Instrumental Analysis
基金
2021年拱北海关关级科技研究项目(2021GK015)。
关键词
分散液液微萃取
超高效液相色谱-四极杆/静电场轨道阱质谱
化妆水
药物残留
dispersive liquid-liquid microextraction
ultra performance liquid chromatographyquadrupole/exactive orbitrap mass spectrometry
lotion
drug residues
作者简介
通讯作者:容裕棠,工程师,研究方向:食品化妆品药物残留分析,E-mail:gdzhrongyutang@163.com。
