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Determination of Clenbuterol in Pork by Solid Phase Extraction Coupling Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

Author: ZhangJianQing
Tutor: ZhangHaiXia
School: Lanzhou University
Course: Analytical Chemistry
Keywords: Clenbuterol Ultra - high performance liquid chromatography tandem mass spectrometry (UPLC-MS-MS) Solid Phase Extraction Three counties , Lanzhou City
CLC: S859.84
Type: Master's thesis
Year: 2010
Downloads: 240
Quote: 1
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Abstract


In recent years, food poisoning incidents continue to occur, the hot issues people are concerned about food safety issues. Clenbuterol is often added to pork feed to increase the lean meat of pork, called clenbuterol. The papers for clenbuterol residues in pork, the establishment of a solid-phase extraction - ultra-high performance liquid chromatography - tandem mass spectrometry, sensitive, rapid, and shipped this method to detect the hydrochloric acid in Lanzhou City, county farmers market pork clent Luo residue. 1. UPLC-MS establishment of clenbuterol detection methods by Waters Acquity UPLC TM BEH C18 column separation of methanol and 0.1% aqueous formic acid mobile phase gradient elution at a flow rate of 0.25 mL / min, and at the same time in multiple reaction monitoring (MRM) mode, optimized cone voltage, collision energy MS conditions. Instrument detection limit of 0.1μg / L, the linear correlation coefficient of 0.9998. 2. Pork in the amount of clenbuterol residues in solid-phase extraction and pre-processing method for collection of pork farmers market base using the Accelerated Solvent Extractor extraction, solid phase extraction clean build enrichment completely simple steps clenbuterol residues pretreatment method. Rapid solvent extraction 6min, 50 ℃ heating to 1500 psi, extract of clenbuterol in pork, also investigated the enrichment capacity of solid phase extraction column of three different filler pork hydrochloride clenbuterol residues, the final choice MCX solid phase extraction column and optimized column speed, elution solvent and elution volume, the pH of the sample solid phase extraction conditions. Optimal experimental conditions, the pork-base, respectively, 0.2, 1.0 and 10.0μg / L spiked recoveries of 78.5% to 98.6%, the relative standard deviation (RSD, n = 3) of 2.9% to 4.3 %, this method can meet the requirements of the detection of trace amounts of clenbuterol residues in pork. Lanzhou City over the county farmers market pork and offal hydrochloride Clenbuterol Residues of pork and offal of the three counties and five District, Lanzhou City, 24 free-market acquisition in November 2008 and May 2009, respectively, its solid phase extraction using established - the ultra-high performance liquid chromatography mass spectrometry analysis of clenbuterol residues. 2008 the clenbuterol Lanzhouxigu District, ancient red zone, Gaolan County, Yuzhong County, Yongdeng County are detected, the detection rate of 33.3%, the highest concentration of 0.15μg/kg . The pork quality has improved, the detection rate fell to 8.3% in 2009. Visceral severe liver residue should remind the general public.

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CLC: > Agricultural Sciences > Livestock, animal medicine,hunting,silkworm,bee > Animal Medicine ( Veterinary Medicine) > Veterinary Pharmacology > Veterinary Toxicology > Chemical residues in animal foods
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