利用LC/MS/MS建立cyenopyrafen於木瓜中殘留分析方法

探討吡唑類殺蟎劑cyenopyrafen 於木瓜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。木瓜基質添加標準品 (0.02, 0.05,0.10 μg/g, n = 5) 測得平均回收率範圍介於82.9 ~ 95.4 % 之間，及相對標準偏差範圍介於1.8 ~ 6.1% 之間。定量極限 (Limit of quantification , LOQ) 為0.01 μg/g。本分析方法具備靈敏度與精確度之效能，可應用於木瓜中cyenopyrafen 殘留量監測管理。另外，探討木瓜基質中cyenopyrafen 冷凍儲存穩定試驗，於木瓜基質添加標準品(0.5, 1.0, 2.0 μg/g, n = 3)，儲存間期為120 天，測得儲存回收率介於75.0 ~ 84.1%之間，及相對標準偏差介於9.4 ~ 11.3% 之間，結果顯示木瓜基質中cyenopyrafen 殘留量在冷凍保存120 天期間可供參考依據。

關鍵字

木瓜；儲存穩定性；液相層析串聯質譜儀； cyenopyrafen

並列摘要

In this study, we developed an effective analytical method for residue analysis of cyenopyrafen, an insecticide that belongs to the pyrazole class of chemical compounds. Specifically, our proposed method uses liquid chromatography tandem mass spectrometry (LC-MS/MS) to quantify cyenopyrafen residues in papaya. In brief, under our method cyenopyrafen residues are extracted from papaya matrices using 0.1% acetic acid in acetonitrile. Chromatographic separation is then performed using an Agilent ZORBAX SB-C18 column in gradient elution mode at 50℃. The mobile phase comprises 0.1% formic acid in 10 mM ammonium formate solution and 0.5% formic acid in acetonitrile at a constant flow rate of 0.3 mL/min. Quantification is performed by reversed phase HPLC with electrospray MS/MS-detection. We found that, at fortified levels of 0.02, 0.05 and 0.10 μg/g cyenopyrafen in papaya, average recovery rate ranged from 82.9 to 95.4%, and relative standard deviation ranged from 1.8 to 6.1%. The limit of quantification (LOQ) was determined to be 0.01 μg/g. Results of this study indicate that our proposed analytical method can easily detect low levels of cyenopyrafen with good precision and sensitivity. Our method could be applied in regulatory and monitoring applications of cyenopyrafen in papaya. We also studied the frozen storage stability of cyenopyrafen residue in papaya. After fortifying papaya with cyenopyrafen concentrations of 0.5, 1.0 and 2.0 μg/g, the samples were placed in a temperature-monitored freezer and stored at approximately -18℃. Fortified recoveries of cyenoprafen in papaya ranged from 75.0 to 84.1% after a storage period of 120 days. These results indicate that cyenopyrafen residues are stable in papaya matrices for at least 120 days when stored under the frozen conditions that are typically employed for actual residue samples. The temperature-monitored freezer at approximately -18℃ for frozen storage. The results of the fortified recoveries ranged from 75.0 to 84.1% after 120 days storage, which indicate that the residues of cyenopyrafen are stable in papaya matrices for at least 120 days when stored under frozen conditions typically employed for actual residue samples.

並列關鍵字

papaya ； storage stability ； LC-MS/MS ； cyenopyrafen

國際替代計量

利用LC/MS/MS建立cyenopyrafen於木瓜中殘留分析方法

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