The study of analytical method for sulfonamide antibiotics and their metabolites in environmental samples

The aim of this study was to develop an analytical method for sulfonamide antibiotics (sulfadiazine, sulfamerazine, sulfamethazine, sulfamethoxazole, sulfathiazole) and their metabolites ($N^4$-acetylsulfadiazine, $N^4$-acetylsulfamerazine, $N^4$-acetylsulfamethazine, $N^4$-acetylsulfamethoxazole, sulfamethoxazole-$N^1$-glucuronide) in environmental samples. The solid phase extraction (SPE) with LC/ESI-MS/MS have been used for the analysis of target compounds, and the recoveries of SPE clean-up were at the range of 12-94% for C18 cartridge, 60-95% for HLB cartridge, 25-123% for MCX cartridge, and 70-90% for tandem HLB/MCX. By established method, detection limit, recovery, and relative standard deviation were 0.001~0.187 ng/mL, 66~115%, and 5~17%, respectively. This method was effective and sensitive to use for the simultaneous determination of sulfonamide antibiotics and their metabolites in environmental samples. Four sulfonamide antibiotics were detected at the range of 0.008~2.153 ng/mL. For metabolites, only $N^4$-acetylsulfamethoxazole was detected, but the concentration was under the MDL level.

환경 시료 중 설폰아미드계 항생제 및 대사체 분석방법 연구

본 연구에서는 동물용 의약품으로 널리 사용되고 환경 중 잔류 가능성이 높은 설폰아미드계 항생제 5종 (sulfadiazine, sulfamerazine, sulfamethazine, sulfamethoxazole, sulfathiazole) 및 대사체 5종($N^4$-acetylsulfadiazine, $N^4$-acetylsulfamerazine, $N^4$--acetylsulfamethazine, N4-acetylsulfamethoxazole, sulfamethoxazole-$N^1$-glucuronide)의 분석방법을 연구하였다. 다양한 전처리 조건을 비교 검토하여 최적의 동시 추출방법과 LC/ESI-MS/MS를 이용한 기기분석 조건을 확립하였다. 카트리지별 추출효율은 C18 카트리지에서 12~94%, HLB 카트리지에서 60-95%, MCX 카트리지에서 25-123%였으며, MCX와 HLB 카트리지를 결합한 방법의 회수율은 70-90%이었다. HLB를 선택하여 확립된 분석방법의 회수율은 66~115%, 상대표준편차 5~17%이었으며, 방법검출한계는 0.001~0.187 ng/mL 였다. 이를 실제 환경시료에 적용한 결과 4종의 설폰아미드 항생제가 0.008~2.153 ng/mL 농도범위로 검출되었으며, 대사체의 경우 $N^4$-acetylsulfamethoxazole이 확인되었으나 검출한계 미만으로 관찰되었다.