Journal
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
Volume 1074, Issue -, Pages 39-45Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.jchromb.2018.01.001
Keywords
Immunoaffinity column; Ultra performance liquid chromatography-tandem mass spectrometry; Methyl-3-quinoxaline-2-carboxylic acid; Animal tissues
Funding
- Natural Science Foundation of Zhejiang Province, China [LY17C200009]
- Scientific and technical tackle key-problem plan project in Henan Province, China [172102310431]
- Zhejiang science and technology program [2016F30022]
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This paper described a reliable and simple method for the selective determination of MQCA in animal tissues using ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). A highly targeted immunoaffinity column was used for sample purification after enzymatic hydrolysis. The purified extracts were analyzed by reversed-phase HPLC-MS/MS in positive ESI and multiple reaction monitoring mode. The calibration curves showed good linearity with correlation coefficient (r(2)) larger than 0.995. The average recoveries at the spiked levels of 0.5, 2.0 and 20 mu g kg(-1) were 90.2% to 103.5% with intra-day and inter-day relatives standard deviations (RSD, n = 6) ranging from 1.8% to 6.7% and 3.5% to 7.6% respectively. The limit of quantification (LOQ) was 0.5 mu g kg(-1), which can fulfil the maximum residue level (MRL) of 4.0 mu g kg(-1) stipulated by the Agricultural Minister of China and the requirement of the confirmatory criteria according to the European Commission Decision 2002/657/EC. The method is sensitive, accurate, convenient and rapid, and has been successfully applied in real samples.
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