农产品中异环丝氨酸及其代谢物的研究分析

Ji Young Kim, Hyo-Jin Kim, Su Jung Lee, Sujin Lim, Gui-Hyun Jang, Guiim Moon, J. M. Lee
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摘要

一种准确、简便的分析方法是测定各种食品基质中异环丝氨酸及其代谢物(SYN549431和SYN548569)残留的必要方法。此外,该方法应满足国内和国际指南(食品药品安全部和食品法典委员会CAC/ GL 40)。采用液相色谱-串联质谱法(LC-MS/MS)测定食品中异环血清及其代谢物残留。为测定残留及其代谢物,取20 mL 0.1%甲酸乙腈,4 g无水硫酸镁,1 g氯化钠,离心(4700 g, 10 min, 4℃)。为了去除干扰和水分,在LC-MS/MS分析前,用c18柱进行d-SPE插装。为了验证该方法,共以五种农产品(糙米、马铃薯、大豆、柑橘和红椒)作为代表性群体。在0.001 ~ 0.05 mg/kg的校准范围内,确定了矩阵匹配的校准曲线,测定系数(r2)≥0.99。检测限为0.003 mg/kg,定量限为0.01 mg/kg。5个样品的平均加样回收率为71.5 ~ 109.8%,精密度小于10%。实验室间验证结果表明,该方法的平均回收率为75.4 ~ 107.0%,变异系数< 19.4%。该方法适用于MFDS、CODEX和EU残留分析指南。因此,该方法可用于日常分析中各种食品基质中残留的测定。
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Study Analysis of Isocycloseram and Its Metabolites in Agricultural Food Commodities
An accurate and easy-to-use analytical method for determining isocycloseram and its metabolites (SYN549431 and SYN548569) residue is necessary in various food matrixes. Additionally, this method should satisfy domestic 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 magnesium sulfate anhydrous and 1 g sodium chloride and centrifuged (4,700 G , 10 min, 4℃). To remove the interferences and moisture, d-SPE cartridge was performed before LC-MS/MS analysis with C 18 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 calibration curves were confirmed with coefficients of determination (R 2 ) ≥ 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 recoveries were 71.5-109.8% and precision was less than 10% for all five samples. In addition, inter-laboratory validation 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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