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She Y.,Chinese Academy of Agricultural Sciences | She Y.,The Tibetan Academy of Agricultural and Animal Husbandry | Liu J.,Chinese Academy of Agricultural Sciences | Wang J.,Chinese Academy of Agricultural Sciences | And 3 more authors.
Analytical Letters | Year: 2010

A novel method has been developed for the rapid separation and determination of 24 Sulfonamides (SAs) in bovine milk by using ultra-performance liquid chromatography tandem quadrupole mass spectrometry (UPLC-MS/MS) in ten minutes. Sulfonamides residues from bovine milk were treated with acetonitrile, followed by homogenizing, ultrasound treating, and centrifuging. The aforementioned procedure is repeated one additional time. A part of the extracts was taken to dryness and defatted twice. The analysis was performed on an Acquity UPLCTM BEH C18 column under the mobile phase which is composed of 0.2% acetic acid in water and acetonitrile. The analytes were detected by multiple reaction monitoring (MRM) in the positive ion scan mode. The calibration curves showed acceptable linearity in the concentration range from 0.2 to 100ngmL1 with correlation coefficients (r2) above 0.992. The mean recoveries of 24 SAs in different standard-spiked levels were in the range of 60.59-116.66%; RSD% was 2.92%~18.64%. Results showed analytical category, separation speed, selectivity, sensitivity, and repeatability of sulfonamides in milk using UPLC-MS/MS that were significantly improved compared to other analytical methods. © Taylor & Francis Group, LLC. Source


She Y.,Chinese Academy of Agricultural Sciences | She Y.,Tibetan Academy of Agricultural and Animal Husbandry | Wang J.,Chinese Academy of Agricultural Sciences | Zheng Y.,Chinese Academy of Agricultural Sciences | And 7 more authors.
Food Chemistry | Year: 2012

A method has been developed for the simultaneous determination of the concentration of nonylphenol (4-NP), nonylphenol monoethoxylates (NP 1EO) and nonylphenol diethoxylates (NP 2EO) in vegetables and crops by liquid chromatography-tandem quadrupole mass spectrometry (HPLC-MS/MS). These target compounds were extracted from vegetable and crop samples with acetonitrile, and then the extracts were cleaned using solid phase extraction with graphitised carbon black tandem primary secondary amine (PSA) cartridges. The MS method enabled highly reliable identification by monitoring the corresponding ammonium adduct [M+NH 4] + in the positive mode for NP 1EO and NP 2EO, and the deprotonated molecule [M-H] - in the negative mode for 4-NP. Recoveries for the spiked samples ranged from 65% to 118%. The limit of detection (LOD) of 4-NP, NP 1EO and NP 2EO was 3, 5 and 0.1 μg kg -1, respectively. This method would be useful for the quick and routine detection of the residues of 4-NP, NP 1EO and NP 2EO in vegetables and crops. © 2011 Elsevier Ltd. All rights reserved. Source

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