LC-MS/MS를 이용한 농산물 중 살균제 Validamycin A의 시험법 개발 = Development of Analytical Method for Detection of Fungicide Validamycin A Residues in Agricultural Products Using LC-MS/MS

다국어 초록 (Multilingual Abstract)

Validamycin A is an aminoglycoside fungicide produced by Streptomyces hygroscopicus that inhibits trehalase. The purpose of this study was to develop a method for detecting validamycin A in agricultural sam-ples to establish MRL values for use in Korea. The validamycin A residues in samples were extracted using methanol/water (50/50, v/v) and purified with a hydrophilic-lipophilic balance (HLB) cartridges. The analyte was quantified and confirmed by liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005~0.5ng) into a blank extract with R2 > 0.99. The limits of detection and quantification were 0.005 and 0.01 mg/kg, respec-tively. For validation validamycin A, recovery studies were carried out three different concentration levels (LOQ, LOQ × 10, LOQ × 50, n = 5) with five replicates at each level. The average recovery range was from 72.5~118.3%, with relative standard deviation (RSD) less than 10.3%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the NIFDS (National Institute of Food and Drug Safety) guide-line (2016). Therefore, the proposed analytical method is accurate, effective and sensitive for validamycin A determi-nation in agricultural commodities.

참고문헌 (Reference)

1 강영운, "축산식품 중 아미노글리코사이드계 항생제 잔류량 분석 및 실태조사" 한국식품과학회 43 (43): 1-5, 2011

2 김찬식, "시료 중 잔류 항생제 분석 방법: III. 기기 분석 방법" 한국물환경학회 32 (32): 649-669, 2016

3 Y. Tao, "Simultaneous determination of 15 aminoglycoside(s)residues in animal derived foods by automated solid-phase extraction and liquid chromatography=tandem mass spectrometry" 135 : 676-683, 2012

4 Chenchen, W., "Simultaneous analysis of kasugamycin and validamycin-A In fruits and vegetables using liquid chromatography-tandem mass spectrometry and consecutive solidphase extraction" 4 : 2016

5 Lee, Y.D., "Practical book of Korea Food Code pesticide residue analysis method" Ministry of Food and Drug Safety 11-15, 2013

6 Maximum Residue Limits, "Maximum Residue Limits (MRLs) List of Agricultural Chemicals in Foods. The Japan Food Chemical Research Foundation"

7 "MRLs in Pesticide" Ministry of Food and Drug Safety 2018

8 박미선, "LC/ESI-MS/MS를 이용한 식육(소, 돼지)중 잔류 phoxim 분석" 대한화학회 55 (55): 626-632, 2011

9 한성희, "LC-MS를 이용한 농산물 중 농업용 항생제 kasugamycin·validamycin 분석" 서울산업대학교 산업대학원 2009

10 조윤제, "LC-MS/MS를 이용한 육류 중 아미노글리코사이드계 항생제9종의 동시분석 및 적용성 검증" 한국식품위생안전성학회 29 (29): 123-130, 2014

11 Using guideline of crop protection agents, "Korea Crop Protection Association"

12 "Guidelines on standard procedures for preparing analysis methods"

13 "Guidelines on good laboratory practice in residue analysis, CAC/GL 40-1993"

14 Michelangelo, A., "Fast and Easy Multiresidue Method Employing Acetonitrile Extraction/partitioning and"Dispersive Solid-Phase Extraction"for the Determination of Pesticide Residues in Produce" 86 (86): 412-431, 2003

15 EU Pesticides database, "European Commission"

16 Yueqiao, L., "Effect of fermentation temperature on validamycin A production by Streptomyces hygroscopicus 5008" 142 : 271-274, 2009

17 Chuanxian, W., "Determination of valdamycin A in agricultural food samples by solid-phase extraction combined with liquid chromatography-atmospheric pressure chemical ionizationtandem mass spectrometry" 169 : 150-155, 2015

18 Clarot, I., "Determination of gentamicin sulfate and related compounds by high-performance liquid chromatography with evaporative light scattering detection" 1031 : 281-287, 2004

19 Na, L., "Determination of Aminoglycoside Fungicide Validamycin A in Rice Plant by Quick, Easy, Cheap, Effective, Rugged, and Safe Approach Using Ultra High performance Liquid Chromatography-Electrospray Ionization-Tandem Mass Spectrometry" 9 : 1736-1744, 2016

20 Tomasz, R., "A review of recent developments and trends in the QuEChERs sample preparation approach" 13 (13): 980-1010, 2015