[Determination of 39 veterinary drug residues in Procambarusclarkii by ultra-high performance liquid chromatography-quadrupole-time of flight mass spectrometry].

An ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF-MS) method was developed for determination of 39 veterinary drugs in Procambarusclarkii. Samples were extracted with acidified acetonitrile and purified with enhanced matrix removal-lipid (EMR-Lipid) adsorbent and graphitized multi-walled carbon nanotubes (GMWNTs). Extracts were analyzed by UHPLC-Q-TOF-MS. Target compounds were screened according to accurate mass, isotopic ratio, and retention time, and confirmed by library search. Target analytes were quantified using the chromatographic peak area of each compound. For each of the drugs of interest, calibration curves were linear in their respective ranges with correlation coefficients greater than 0.99. The limits of quantification (LOQs) were 3-15 µg/kg. The recoveries for target compounds spiked in Procambarusclarkii ranged from 62.4% to 105.8%, with relative standard deviations (RSDs) ranging from 2.5% to 13.5%. This method is simple, rapid, accurate, and suitable for simultaneous determination of 39 veterinary drugs, including sulfonamides, quinolones, and triphenylmethane, extracted from Procambarusclarkii.

[Rapid determination of 204 pesticide residues in tea by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry].

An analytical method was established for the simultaneous determination of 204 pesticide residues in tea by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UPLC-Q-TOF/MS). The samples were extracted with acetonitrile, and cleaned-up by solid phase extraction (SPE) with a Carb-PSA cartridge, eluted with acetonitrile-toluene (3:1, v/v), determined by UPLC-Q-TOF/MS and quantified by external standard method. A data base of the accurate mass numbers and a library which contains the 204 pesticides were established. The automatic retrieval of detection results was carried on according to the characteristics of the compound, such as accurate mass, retention time, isotopic ratio, and so on. Based on the above results, the qualitative identifications of the 204 pesticides were accomplished without the contrast of standard substances. The results indicated that this method can be used to determine the 204 pesticides in tea. At the three spiked levels of 10, 20, 50 µg/kg, mean recoveries for the 204 pesticides in tea were between 68. 1% and 117. 2%, with the relative standard deviations (RSDs) ranging from 3.1% to 18.9%. The limits of quantification for the 204 pesticides were lower than 10 µg/kg. The method has been applied to four positive samples, and the results generally accord with the detection results by the method of GB/T 23205-2008. This method has the characteristics of high efficiency, as well as high sensitivity and accuracy, which can meet the requirement of the determination of the 204 pesticides in tea.