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Korean J. Vet. Serv. 2004; 27(1): 17-29

Published online March 1, 2004

© The Korean Socitety of Veterinary Service

HPLC와 LC/MS에 의한 식육내 잔류 설파제의 동시 분석법

정봉수;박준조;금모래;김인경;박병옥;한정희;

경기도축산위생연구소;경기도축산위생연구소;경기도축산위생연구소;경기도축산위생연구소;경기도축산위생연구소;강원대학교 수의학과;

Simultaneous analysis of sulfonamides in beef and pork by high performance liquid chromatography and electrospray ionization mass spectrometry

정봉수;박준조;금모래;김인경;박병옥;한정희;

Correspondence to : 경기도축산위생연구소

Abstract

A multiresidual analysis was performed to determine 12 sulfonamides(sulfacetamide, sulfadiazine, sulfisomidine, sulfathiazole, sulfapyridine, sulfamerazine, sulfamethazine, sulfamonomethoxine, sulfisoxazole, sulfamethoxazole, sulfaquinoxaline, and sulfadimethoxine) in beef and pork simultaneously. The multiresidual analysis for the sulfonamides currently used was able to analyze 5 kinds of sulfonamides at the same time. The method of this 12 sulfonamides multiresidual analysis in this study was matrix solid-phase dispersion(MSPD) by high performance liquid chromatography (HPLC) and liquid chromatography mass spectrometry (LC/MS). The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM: Ethylacetate(3:1), DCM:EA(9:1). Also, samples (84 beef and 205 pork samples) which were positive by EEC-4 plate test from 2001 to 2003 were tested to investigate the kinds of sulfonamides using HPLC. The results from the study were as follows; 1. The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM:Ethylacetate(3:1), DCM:EA(9:1). The method of extraction solvent with DCM:ethyl acetate(9:1) was the most excellent(87.7∼99.3%) in separation and reappearance. 2. In the LC/MS analysis. of sulfonamides, signal to noise ratio was showed relatively high in the positive mode and special ion in the quality analysis was determined via [M+H]$^$+/ and m/z 156. A spectrum of sulfonamides was showed from all 12 sulfonamides. 3. The samples positive by the EEC-4 plate, a screening test method, were categorized by sulfonamides through Charm II and confirmed the kinds of sulfonamides through HPLC. 1) Among 84 beef samples positive by EEC-4 plate, 20 samples were positive by Charm II and identified as 7 sulfamethazine, 9 sulfadimethoxine, 1 sulfamonomethoxine and 3 unknown status. 2) Among 205 pork samples positive by EEC-4 plate, 42 samples were positive by Charm II and identified as 19 sulfamethazine, 1 sulfadimethoxine, 4 sulfamonomethoxine and 5 unknown status.

Keywords Sulfanilamides,Electrospray ionization mass spectrometry,Fraction ion,

Article

Research Article

Korean J. Vet. Serv. 2004; 27(1): 17-29

Published online March 1, 2004

Copyright © The Korean Socitety of Veterinary Service.

HPLC와 LC/MS에 의한 식육내 잔류 설파제의 동시 분석법

정봉수;박준조;금모래;김인경;박병옥;한정희;

경기도축산위생연구소;경기도축산위생연구소;경기도축산위생연구소;경기도축산위생연구소;경기도축산위생연구소;강원대학교 수의학과;

Simultaneous analysis of sulfonamides in beef and pork by high performance liquid chromatography and electrospray ionization mass spectrometry

정봉수;박준조;금모래;김인경;박병옥;한정희;

Correspondence to:경기도축산위생연구소

Abstract

A multiresidual analysis was performed to determine 12 sulfonamides(sulfacetamide, sulfadiazine, sulfisomidine, sulfathiazole, sulfapyridine, sulfamerazine, sulfamethazine, sulfamonomethoxine, sulfisoxazole, sulfamethoxazole, sulfaquinoxaline, and sulfadimethoxine) in beef and pork simultaneously. The multiresidual analysis for the sulfonamides currently used was able to analyze 5 kinds of sulfonamides at the same time. The method of this 12 sulfonamides multiresidual analysis in this study was matrix solid-phase dispersion(MSPD) by high performance liquid chromatography (HPLC) and liquid chromatography mass spectrometry (LC/MS). The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM: Ethylacetate(3:1), DCM:EA(9:1). Also, samples (84 beef and 205 pork samples) which were positive by EEC-4 plate test from 2001 to 2003 were tested to investigate the kinds of sulfonamides using HPLC. The results from the study were as follows; 1. The recovery rate of the materials was measured by MSPD method with 3 different extraction solvents; Dichloromethane, DCM:Ethylacetate(3:1), DCM:EA(9:1). The method of extraction solvent with DCM:ethyl acetate(9:1) was the most excellent(87.7∼99.3%) in separation and reappearance. 2. In the LC/MS analysis. of sulfonamides, signal to noise ratio was showed relatively high in the positive mode and special ion in the quality analysis was determined via [M+H]$^$+/ and m/z 156. A spectrum of sulfonamides was showed from all 12 sulfonamides. 3. The samples positive by the EEC-4 plate, a screening test method, were categorized by sulfonamides through Charm II and confirmed the kinds of sulfonamides through HPLC. 1) Among 84 beef samples positive by EEC-4 plate, 20 samples were positive by Charm II and identified as 7 sulfamethazine, 9 sulfadimethoxine, 1 sulfamonomethoxine and 3 unknown status. 2) Among 205 pork samples positive by EEC-4 plate, 42 samples were positive by Charm II and identified as 19 sulfamethazine, 1 sulfadimethoxine, 4 sulfamonomethoxine and 5 unknown status.

Keywords: Sulfanilamides,Electrospray ionization mass spectrometry,Fraction ion,

KJVS
Mar 30, 2024 Vol.47 No.1, pp. 1~7

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Korean Journal of
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