以液相層析串聯質譜儀建立亞喜芬、氟硫滅、依速隆於農產品中殘留檢驗方法

Establishment of an LC-MS/MS Analytical Method to Assess Acifluorfen, Flusulfamide and Imazosulfuron Residues in Agricultural Products

莊瑋臻(Wei-Chen Chuang) ； 黃鎮華(Chen-Hua Huang) ； 徐慈鴻(Tsyr-Horng Shyu) ； 林韶凱(Shao-Kai Lin)

《臺灣農藥科學》 13期 (2022/12) Pp. 59-78

https://doi.org/10.6671/TPS.202212_(13).04

摘要

本研究係開發亞喜芬、氟硫滅、依速隆於農產品中殘留檢驗方法，檢驗方法參考「食品中殘留農藥檢驗方法－多重殘留分析方法（六）」（2021年12月30日修正，TFDAP0007.02）進行分析，萃取液分別以液相層析串聯質譜儀進行定性及定量，試驗材料以甘藍、芥藍、白米及綠茶進行檢驗方法確效，於蔬菜樣品中添加濃度為0.01及0.05 μg/g、白米添加濃度為0.02及0.10 μg/g、綠茶添加濃度為0.05及0.25 μg/g，進行同日內與異日間之評估，亞喜芬於同日內（intra-day）平均回收率介於89.8～112.4%，相對標準偏差（relative standard deviation, RSD）介於3.4～7.7%，異日間（inter-day）平均回收率介於88.4～104.7%，RSD介於2.3～9.0%；氟硫滅於同日內平均回收率介於89.7～111.4%，RSD介於1.3～4.0%，異日間平均回收率介於90.9～108.8%，RSD介於2.2～4.4%；依速隆於同日內平均回收率介於74.3～102.6%，RSD介於2.2～10.1%；異日間平均回收率介於82.2～99.4%，RSD介於4.3～11.8%。上述3種藥劑的定量極限於蔬菜可達0.01 μg/g、白米可達0.02 μg/g、綠茶可達0.05 μg/g。本方法期能作為衛福部食品藥物管理署制定檢驗方法之參考依據，未來將運用於進、出口及市售產品中檢測殘留情形，為食安把關。

關鍵字

亞喜芬 ； 氟硫滅 ； 依速隆 ； 液相層析串聯質譜儀 ； 檢驗方法確效

並列摘要

Many pesticides have established maximum residue limits; however, some still lack methods to test for these residues. This study established an analytical method for testing acifluorfen, flusulfamide and imazosulfuron residues in agricultural products. Our method analyzes agricultural extracts qualitatively and quantitatively using a liquid chromatography tandem mass spectrometer and was developed using the "Method of Test for Pesticide Residues in Foods-Multiresidue Analysis (6)" (TFDAP0007.02) as a reference. We validated our analytical method using cabbage, kale, rice and green tea as test materials. Vegetable samples were fortified at levels of 0.01 and 0.05 μg/g. Rice samples were fortified at levels of 0.02 and 0.10 μg/g. Green tea samples were fortified at levels of 0.05 and 0.25 μg/g. For acifluorfen, average inter-day recovery rates ranged from 88.4~104.7% (relative standard deviation [RSD]: 2.3~9.0%), and average intra-day recovery rates ranged from 89.8~112.4% (RSD: 3.4~7.7%). For flusulfamide, average inter-day recovery rates ranged from 90.9~108.8% (RSD: 2.2~4.4%), and average intra-day recovery rates ranged from 89.7~111.4% (RSD: 1.3~4.0%). For imazosulfuron, average inter-day recovery rates ranged from 82.2~99.4% (RSD: 4.3~11.8%), and average intra-day recovery rates ranged from 74.3~102.6% (RSD: 2.2~10.1%). Limit of quantification (LOQ) values for the three pesticides were 0.01 μg/g in vegetables, 0.02 μg/g in rice and 0.05 μg/g in green tea. The analytical method developed in this study can be applied to detect acifluorfen, flusulfamide and imazosulfuron residues in imported, exported, and other commercially available products, thereby safeguarding food safety. Our method can also serve as a reference in the development of additional testing methods by the Food and Drug Administration, Ministry of Health and Welfare.

並列關鍵字

Acifluorfen ； Flusulfamide ； Imazosulfuron ； liquid chromatography tandem mass spectrometer ； method validation