LC-MS/MS를 이용한 농산물 중 Streptomycin 및 Dihydrostreptomycin 동시시험법 개발 = Development of Simultaneous Analytical Method for Streptomycin and Dihydrostreptomycin Detection in Agricultural Products Using LC-MS/MS

다국어 초록 (Multilingual Abstract)

A method was developed for the simultaneous detection of an antibiotic fungicide, streptomycin, and its metabolite (dihydrostreptomycin) in agricultural products using liquid chromatography-tandem mass spec-trometry (LC-MS/MS). The samples were extracted using methanol adjusted to pH 3 using formic acid, and purified with a HLB (Hydrophilic lipophilic balance) cartridge. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.001 to 0.1 mg/kg, and linearity of five agricultural products (hulled rice, potato, soybean, mandarin, green pepper), with coefficients of determination (R2) ≥ 0.9906, for streptomycin and dihydrost-reptomycin. The mean recoveries at three fortification levels (LOQ, LOQ × 10, LOQ × 50, n = 5) were from 72.0~116.5% and from 72.1~116.0%, and relative standard deviations were less than 12.3% and 12.5%, respectively. The limits of quantification (LOQ) were 0.01 mg/kg, which are satisfactory for quantification levels corresponding with the Positive List System. All optimized results satisfied the criteria ranges requested in the Codex guidelines and the Food Safety Evaluation Department guidelines. The present study could serve as a reference for the establishment of maximum residue limits and be used as basic data for detection of streptomycin and dihydrostreptomycin in food.

참고문헌 (Reference)

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

2 Jadhav, M. R., "Validation of a residue analysis method for streptomycin and tetracycline and their food safety evaluation in pomegranate(Punica granatum L. )" 61 : 8491-8498, 2013

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

4 Millership, J. S., "The use of hydrophilic lipophilic balanced(HLB)copolymer SPE cartridges for the extraction of diclofenac from small volume paediatric plasma samples" 25 : 871-879, 2001

5 Korean Society for Molecular and Cellular Biology, "Streptomycin"

6 Chemicalize, "Streptomycin"

7 United States Environmental Protection Agency, "Regulation of Pesticide Residues on Food"

8 EU Reference Laboratory for pesticides requiring Single Residue Methods, "Quick Method for the Analysis of numerous Highly Polar Pesticides in Foods of Plant Origin via LC-MS/MS involving Simultaneous Extraction with Methanol (QuPPe-Method)"

9 Ministry of Food and Drug Safety, "Pesticide analytical residues manual in food code"

10 The Joint FAO/WHO Expert Committee on Food Additives, "Online Edition: “Residues of some veterinary drugs in foods and animals”"

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

12 Ministry of Food and Drug Safety, "MRLs in Veterinary drugs"

13 Ministry of Food and Drug Safety, "MRLs in Pesticide"

14 심영은, "LC-MS/MS를 이용한 벌꿀 중 스트렙토마이신 분석" 한국분석과학회 21 (21): 424-431, 2008

15 Ministry of Food and Drug Safety, "Korea food code"

16 Ministry of Food and Drug Safety, "Korea food code"

17 Gremilogianni, A. M., "Hydrophilic interaction vs ion pair liquid chromatography for the determination of streptomycin and dihydrostreptomycin residues in milk based on mass spectrometric detection" 1217 : 6646-6651, 2010

18 Kumar, P., "Hydrophilic interaction chromatography for the analysis of aminoglycosides" 35 : 498-504, 2011

19 Ministry of Food and Drug Safety, "Guidelines on standard procedures for preparing analysis method"

20 CODEX Alimentarius Commission, "Guidelines on good laboratory practice in residue analysis. CAC/GL 40-1993"

21 European Commission, "EU Pesticides database"

22 Chemicalize, "Dihydrostreptomycin"

23 Encyclopedia of Life Science, "Dihydrostreptomycin"

24 Oliveira, R. C. de, "Development and validation of an LC-APCI-MS-MS analytical method for the determination of streptomycin and dihydrostreptomycin residues in milk" 47 : 756-761, 2009

25 도정아, "Determination of streptomycin in kiwifruit samples using LC-ESI-MS/MS" 한국분석과학회 28 (28): 299-307, 2015

26 Bruijnsvoort, M., "Determination of streptomycin and dihydrostreptomycin in milk and honey by liquid chromatography with tandem mass spectrometry" 1058 : 137-142, 2004

27 Bohm, D. A., "Confirmatory method for the determination of streptomycin and dihydrostreptomycin in honey by LC-MS/MS" 29 : 189-196, 2012

28 Ko A. Y., "A modified QuEChERS method for simultaneous determination of flonicamid and its metabolites in paprika using tandem mass spectrometry" 157 : 413-420, 2014