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1.
Se Pu ; 36(7): 634-642, 2018 Jul 08.
Article in Chinese | MEDLINE | ID: mdl-30136535

ABSTRACT

An ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry (UPLC-Q Orbitrap HRMS) method was developed for the rapid determination of 48 contaminant residues in food plastic packaging materials. The samples were extracted with methanol using microwave-assisted extraction. The separation of the 48 contaminants was performed on a CAPCELL PAK MG Ⅱ C18 column (150 mm×2.0 mm, 5 µm) with gradient elution. Methanol (containing 0.04% (v/v) formic acid) and water (containing 0.04% (v/v) formic acid and 20 mmol/L ammonium acetate) were used as mobile phases. The compounds were detected under the full scan/date dependent-MS/MS (Full MS/dd-MS2) mode with a heated electrospray ionization (HESI) source. The calibration curves were linear with correlation coefficients no less than 0.9950. The limits of detection (LODs) ranged from 0.1 to 1.0 µg/kg. The average spiked recoveries of the 48 target compounds were between 71.2% and 108.8%, with relative standard derivations (RSDs) ranging from 2.2% to 11.8% (n=6). Compared to previous methods, this method has advantages of simpler sample preparation and higher sensitivity.


Subject(s)
Food Contamination/analysis , Food Packaging , Plastics/analysis , Calibration , Chromatography, High Pressure Liquid , Limit of Detection , Microwaves , Static Electricity , Tandem Mass Spectrometry
2.
Se Pu ; 36(2): 114-124, 2018 Feb 08.
Article in Chinese | MEDLINE | ID: mdl-29582597

ABSTRACT

An ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry (UPLC-Q Orbitrap HRMS) method was developed for the rapid screening of 25 drug residues in aquatic products by the application of a novel enhanced matrix removal of lipids (EMR-Lipid). The samples were extracted with acetonitrile, cleaned-up with EMR-Lipid, and salted out with 3.0 g sodium chloride and 3.0 g sodium sulfate. The separation of the 25 drug residues was performed on an ACQUITY UPLC BEH C18 column (100 mm×2.1 mm, 1.7 µm) with gradient elution. Acetonitrile containing 0.1% (v/v) formic acid and 0.1% (v/v) formic acid aqueous solution were used as mobile phases. The compounds were detected by Full scan/date dependent MS/MS (Full MS/dd-MS2) via heated electrospray ionization (HESI) source. The calibration curves were linear with correlation coefficients (r) greater than 0.997. The limits of detection (LODs) ranged from 0.1 µg/kg to 1.0 µg/kg. The average spiked recoveries of the 25 target compounds were between 70.1% and 108.9% with relative standard derivations (RSDs) from 2.1% to 13.8%. Compared with the previous methods, this method has characteristics of simpler sample preparation and higher sensitivity.


Subject(s)
Chromatography, High Pressure Liquid , Drug Residues/analysis , Mass Spectrometry , Seafood/analysis , Calibration , Limit of Detection
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