Study Analysis of Isocycloseram and Its Metabolites in Agricultural Food Commodities
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An accurate and easy-to-use analytical method for de-termining isocycloseram and its metabolites (SYN549431 and SYN548569) residue is necessary in various food matrixes. Additionally, this method should satisfy domes-tic and international guidelines (Ministry of Food and Drug Safety and Codex Alimentarius Commission CAC/ GL 40). Liquid Chromatography-Tandem Mass Spectro- metry (LC-MS/MS) was used to determine the isocyclo- seram and its metabolites residue in foods. To determine the residue and its metabolites, a sample was extracted with 20 mL of 0.1% formic acid in acetonitrile, 4 g magne-sium sulfate anhydrous and 1 g sodium chloride and cen-trifuged (4,700 G, 10 min, 4℃). To remove the interferences and moisture, d-SPE cartridge was performed be-fore LC-MS/MS analysis with C18 column. To verify the method, a total of five agricultural commodities (hulled rice, potato, soybean, mandarin, and red pepper) were used as a representative group. The matrix-matched cali-bration curves were confirmed with coefficients of deter-mination (R2) ≥ 0.99 at a calibration range of 0.001-0.05 mg/kg. The limits of detection and quantification were 0.003 and 0.01 mg/kg, respectively. Mean average recov-eries were 71.5-109.8% and precision was less than 10% for all five samples. In addition, inter-laboratory vali-dation testing revealed that average recovery was 75.4- 107.0% and the coefficient of variation (CV) was below 19.4%. The method is suitable for MFDS, CODEX, and EU guideline for residue analysis. Thus, this method can be useful for determining the residue in various food ma-trixes in routine analysis.
Abstract
An accurate and easy-to-use analytical method for de-termining isocycloseram and its metabolites (SYN549431 and SYN548569) residue is necessary in various food matrixes. Additionally, this method should satisfy domes-tic and international guidelines (Ministry of Food and Drug Safety and Codex Alimentarius Commission CAC/ GL 40). Liquid Chromatography-Tandem Mass Spectro- metry (LC-MS/MS) was used to determine the isocyclo- seram and its metabolites residue in foods. To determine the residue and its metabolites, a sample was extracted with 20 mL of 0.1% formic acid in acetonitrile, 4 g magne-sium sulfate anhydrous and 1 g sodium chloride and cen-trifuged (4,700 G, 10 min, 4℃). To remove the interferences and moisture, d-SPE cartridge was performed be-fore LC-MS/MS analysis with C18 column. To verify the method, a total of five agricultural commodities (hulled rice, potato, soybean, mandarin, and red pepper) were used as a representative group. The matrix-matched cali-bration curves were confirmed with coefficients of deter-mination (R2) ≥ 0.99 at a calibration range of 0.001-0.05 mg/kg. The limits of detection and quantification were 0.003 and 0.01 mg/kg, respectively. Mean average recov-eries were 71.5-109.8% and precision was less than 10% for all five samples. In addition, inter-laboratory vali-dation testing revealed that average recovery was 75.4- 107.0% and the coefficient of variation (CV) was below 19.4%. The method is suitable for MFDS, CODEX, and EU guideline for residue analysis. Thus, this method can be useful for determining the residue in various food ma-trixes in routine analysis.
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