利用LC-MS/MS建立oxathiapiprolin於葡萄中殘留分析方法

探討殺菌劑oxathiapiprolin於葡萄中殘留分析方法的建立，以含1%醋酸的氰甲烷溶液作為萃取溶液，及利用液相層析串聯式質譜儀（Liquid Chromatograph-Tandem Mass Spectrometry, LC-MS/MS）進行測定。葡萄基質添加標準品（0.02,0.05,0.1μg/g,n=5）測得平均回收率範圍介於91.0～98.6%之間，及相對標準偏差範圍介於1.1～3.0%。定量極限（Limit of quantification, LOQ）為0.01μg/g。本分析方法具備靈敏度與精確度之效能，可應用於葡萄中oxathiapiprolin殘留量監測管理。另外，探討葡萄基質中oxathiapiprolin冷凍儲存穩定試驗，於葡萄基質添加標準品（0.5,1.0,2.0μg/g, n=3），儲存間期為83天，測得儲存回收率介於84.6～90.2%之間，及相對標準偏差介於1.2～3.9%之間，結果顯示葡萄基質中oxathiapiprolin殘留量在冷凍保存83天期間可供參考依據。

關鍵字

液相層析串聯質譜儀； oxathiapiprolin ；葡萄；儲存穩定性

並列摘要

In this study, we developed an effective analytical method for the residue analysis of oxathiapiprolin, an insecticide that belongs to the diamide family of chemical compounds. Specifically, our proposed method employs liquid chromatography tandem mass spectrometry (LC-MS/MS) to quantify oxathiapiprolin residues in grapes. First, oxathiapiprolin residues are extracted from grape matrices using 1% acetic acid in acetonitrile. Then, chromatographic separation is then performed using an Agilent ZORBAX SB-C18 column in gradient elution mode at 50°C. For this, the mobile phase comprises 0.1% formic acid in 10.1 mM ammonium formate solution and 0.5% formic acid in acetonitrile, and the flow rate is maintained at a constant 0.3 mL/min. Quantification is performed by reversed-phase HPLC with electrospray MS/MS-detection. We found that, when grapes were fortified at levels of 0.02, 0.05, and 0.1 μg/g oxathiapiprolin, average recovery rates ranged from 91.0 to 98.6%, and relative standard deviations ranged from 1.1 to 3.0%. The limit of quantification (LOQ) was found to be 0.01 μg/g. Results of this study indicate that our proposed analytical method (1) can easily detect low levels of oxathiapiprolin and (2) has good precision and sensitivity. Our method could be applied to benefit regulatory and monitoring applications pertaining to oxathiapiprolin in grapes. We also investigated the frozen storage stability of oxathiapiprolin residue in grapes. After fortifying grapes with 0.5, 1.0 and 2.0 μg/g oxathiapiprolin, samples were placed in a temperature-monitored freezer and maintained at approximately -18°C. After 83 days, recovery rates ranged from 84.6 to 90.2%, which indicates that oxathiapiprolin residues are stable in grape matrices for at least 83 days when stored under the frozen conditions which are typically employed for actual residue samples.

並列關鍵字

LC-MS/MS ； oxathiapiprolin ； grape ； storage stability

國際替代計量

利用LC-MS/MS建立oxathiapiprolin於葡萄中殘留分析方法

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