Article pubs.acs.org/JAFC
Rapid and Easy Multiresidue Method for the Analysis of Antibiotics in Meats by Ultrahigh-Performance Liquid Chromatography− Tandem Mass Spectrometry Takahiro Yamaguchi,† Masahiro Okihashi,† Kazuo Harada,*,§,# Kotaro Uchida,† Yoshimasa Konishi,† Keiji Kajimura,† Kazumasa Hirata,§,# and Yoshimasa Yamamoto†,# †
Osaka Prefectural Institute of Public Health, 1-3-69 Nakamichi, Higashinari-ku, Osaka 537-0025, Japan Graduate School of Pharmaceutical Sciences, Osaka University, 1-6 Yamadaoka, Suita, Osaka 565-0871, Japan # Global Collaboration Center, Osaka University, 2-7 Yamadaoka, Suita, Osaka 565-0871, Japan §
ABSTRACT: This study involved the development of a multiresidue method for the rapid analysis of 43 antibiotics in meats using ultrahigh-performance liquid chromatography−tandem mass spectrometry. This method was performed using dispersivesolid phase extraction, which is able to analyze 20 samples within 2 h. All compounds were determined simultaneously on a C18 separation column with gradient elution. Validation of the analytical method was performed by carrying out linearity, limit of quantification (LOQ), accuracy, precision, and recovery tests in different meat products. The validation criteria were set according to AOAC International and Japanese validation guidelines. The linearity of each compound was almost the coefficient of determination (r2) > 0.98. The LOQs of all tested antibiotics were 0.99 for almost all target compounds, except sulfapyridine and sulfadoxine, which were >0.98. The LOQs were estimated from the signal-to-noise ratio (S/N) (Table 2). S/N was determined at the peak height of beef, pork, and chicken samples spiked with 1 ng/mL target compounds. The background noise was estimated near each analyte peak. Precision and accuracy were performed according to the guidelines of AOAC International and the Japanese Ministry of Health, Labor and Welfare.26,27 Recovery tests of 43 antibiotic residues from beef, pork, and chicken were performed at two different concentration levels, 10 and 100 μg/kg, in duplicate by three persons on two separate days. No interfering peaks were detected near the retention time of the analytes. The validation data were evaluated on the basis of recoveries of 70−125%, RSDr of
