利用LC-MS/MS建立propyrisulfuron於糙米中殘留分析方法

Novel Method for the Determination of Propyrisulfuron Residues in Rice Using LC-MS/MS

許菁菁(Jing-Jing Syu) ； 陳惠姬(Hui-Chi Chen) ； 徐慈鴻(Tsyr-Horng Shyu)

《臺灣農藥科學》 3期 (2017/12) Pp. 25-37

https://doi.org/10.6671/TPS/2017.003.02

摘要

探討尿素系除草劑propyrisulfuron於糙米中殘留分析方法的建立，以含有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。糙米基質添加標準品(0.04, 0.1, 0.2 μg/g, n = 9)測得平均回收率範圍介於83.4～97.8%之間，及相對標準偏差範圍介於7.0～12.1%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，可應用於稻米中propyrisulfuron殘留量監測管理。另外，探討糙米基質中propyrisulfuron冷凍儲存穩定試驗，於糙米基質添加標準品(0.5, 1.0, 2.0 μg/g, n = 3)，儲存間期為70天，測得儲存回收率範圍介於105.7～114.7%之間，及相對標準偏差範圍介於2.0～4.1%之間，結果顯示糙米基質中propyrisulfuron殘留量在冷凍保存70天期間呈現穩定狀態。

關鍵字

液相層析串聯式質譜儀 ； 糙米 ； 儲存穩定 ； propyrisulfuron

並列摘要

An effective analytical method for the residue analysis of propyrisulfuron was studied. Propyrisulfuron is a herbicide, which belongs to the chemical class of urea compound. A liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for the determination of propyrisulfuron in rice. Residue of propyrisulfuron in rice matrices was extracted with 0.1% acetic acid in acetonitrile. Chromatographic separation was achieved on an Agilent ZORBAX SB-C18 chromatography column in gradient elution mode at 50℃. Mobile phase using 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. The quantification is performed by reversed phase HPLC with electrospray MS/MS-detection. At fortified levels of 0.04, 0.1 and 0.2 μg/g propyrisulfuron in rice, it was shown that average recovery rate ranged from 83.4 to 97.8%, with a relative standard deviation ranged from 7.0 to 12.1%. The limit of quantification (LOQ) was found to be 0.01 μg/g. Based on the results of this study, propyrisulfuron is easy to detect with good precision and sensitivity at low levels. This analytical method will be applied for the relevant residue monitoring and regulation. In addition, the frozen storage stability of propyrisulfuron residue in rice was studied. After fortifying rice with propyrisulfuron at concentrations of 0.5, 1.0 and 2.0 μg/g, the samples were placed in a temperature-monitored freezer at approximately -18℃ for frozen storage. The results of the fortified recoveries ranged from 105.7 to 114.7% after 70 days storage, which indicate that residues of propyrisulfuron are stable in rice matrices for at least 70 days when stored under frozen conditions typically employed for actual residue samples.

並列關鍵字

LC-MS/MS ； rice ； storage stability ； propyrisulfuron