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KMID : 0881720190340030227
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Journal of Food Hygiene and Safety
2019 Volume.34 No. 3 p.227 ~ p.234
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Development and Validation of the Analytical Method for Oxytetracycline in Agricultural Products using QuEChERS and LC-MS/MS
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Cho Sung-Min
Do Jung-Ah
Lee Han-Sol
Park Ji-Su
Shin Hye-Sun
Jang Dong-Eun
Cho Myong-Shik
Jung Yong-Hyun
Lee Kang-Bong
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Abstract
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An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using MgSO 4 (anhydrous magnesium sulfate), PSA (primary secondary amine), C 18 (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels (0.001~0.25 μg/mL) and coefficient of determination (r2 ) was above 0.99. Recovery results at three concentrations (LOQ, 10×LOQ, and 50×LOQ, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.
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KEYWORD
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Pesticide, Oxytetracycline, Fungicide, Analytical method, Agricultural product, , LC-MS/MS
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