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| Rapid Screening of 139 Kinds of Drug Residues in Lotion by Dispersive Liquid－Liquid Microextraction/Ultra Performance Liquid Chromatography－Quadrupole/Exactive Orbitrap Mass Spectrometry |
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| DOI： |
| KeyWord:dispersive liquid－liquid microextraction ultra performance liquid chromatography－quadrupole/exactive orbitrap mass spectrometry lotion drug residues |
| Author | Institution |
| RONG Yu-tang，ZHANG Xian-chen，DENG Xiao-ying，WU Jie-shan，LIU Qiong-yu，CAI Jie，WENG Fu-liang |
1. Technology Center of Gongbei Customs，Zhuhai ，China; 2. Technology Center of Zhongshan Customs，Zhongshan ，China |
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| Abstract: |
| 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，50 μL of extraction agent tetrachloroethane，300 μL 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，2.2 μm） column．By using Q－Exactive 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 10－1 000 ng/mL（r > 0.99）．The detection limits were 10－30 μg/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. |
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