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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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