구.농수식품
건국대학교 수의과대학
Abstract
Weijia Zhenga, 1, Kyung-Hee Yooa, 1, A.M. Abd El-Atyb, c,*, Da-Hee Parka, Jeong-Min Choia, Seong-Kwan Kima , Young-Sun Kanga, d, Hongxia Zhange, Ahmet Hacımüftüoğluc, Alaa El-Din Bekhitf, Jing Wangg, Jae-Han Shimh, Ho-Chul Shina, *
a Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul 143-701, Republic of Korea
b Department of Pharmacology, Faculty of Veterinary Medicine, Cairo University, 12211 Giza, Egypt
c Department of Medical Pharmacology, Medical Faculty, Ataturk University, 25240 Erzurum, Turkey
d Department of Biomedical Science and Technology, Konkuk University, Seoul 143-701, Republic of Korea
e State Key Laboratory of Biobased Material and Green Papermaking, College of Food Science and Engineering, Qilu University of Technology, Shandong Academy of Science, P.O. Box 250353, Jinan, Shandong, China
f Department of Food Science, University of Otago, PO Box 56, Dunedin, New Zealand
g Key Laboratory of Agro-Product Quality and Safety, Institute of Quality Standard and Testing Technology for Agro-Product, Chinese Academy of Agricultural Sciences, 100081 Beijing, PR China
h Natural Products Chemistry Laboratory, College of Agriculture and Life Sciences, Chonnam National University, 300 Yongbong-dong, Buk-gu, Gwangju 500-757, Republic of Korea
1 The first two authors contributed equally to this article.
*Correspondingauthors
Abstract
This work describes a simple screening protocol for quantification of carbasalate calcium derived metabolites, acetylsalicylic acid (ASA) and salicylic acid (SA), in animal and aquatic food matrices using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The analytes were extracted from porcine muscle, milk, egg, shrimp, eel, and flatfish using acetonitrile, with the addition of formic acid as well as trifluoroacetic acid, followed by liquid-liquid purification with saturated n-hexane. A reverse-phase analytical column was employed with a mobile phase comprising (A) 1?mM ammonium acetate in distilled water and (B) methanol to achieve the best chromatographic separation. Matrix-matched calibration curves (R2 ≥ 0.9817) were constructed using six concentrations of 5, 10, 20, 30, 40, and 50?μg/kg in porcine muscle, milk, egg, shrimp, eel, and flatfish matrices. The calculated limits of quantification (LOQ) were 10 and 7 μg/kg, for ASA and SA, respectively. Recoveries of 67 to 102% with relative standard deviations (RSDs) of ≤9.0% (intra-day and inter-day) were obtained for all matrices at four spiking concentrations (5, 10, 20, and 50 μg/kg). The method was feasibly applied for monitoring market samples. In conclusion, the developed method is versatile, accurate, and precise for detecting and quantifying acetylsalicylic acid and salicylic acid residues in animal-derived foods meant for human consumption.
Keywords : Carbasalate calcium, Acetylsalicylic acid, Salicylic acid, Animal-derived foods, Residue, Liquid chromatography-tandem mass, spectrometry
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