成品農藥中植物生長調節劑多重檢測分析方法之建立

植物生長調節劑為具有植物荷爾蒙功能之天然或人工合成物質，可調節植物生長與發育。依據農藥管理法第七條第二款及農藥標準規格準則第三條附表六，成品農藥中摻雜巴克素、移植生長素、單克素、番茄生長素、開寧激素、福芬素、氟氯比7種植物生長調節劑有效成分之限量基準為0.01%、摻雜快克草之限量基準依不同劑型為3%或0.1%、8種植物生長調節劑之檢測極限為0.001%。目前檢驗成品農藥摻雜該等植物生長調節劑有效成分時，皆為單一成分分析方法，本研究利用液相層析串聯質譜儀開發多重分析方法，可同時分析成品農藥中8種植物生長調節劑。供試成品農藥以甲醇為稀釋溶劑，經超音波振盪萃取，再經濾膜過濾後以液相層析串聯質譜儀搭配多重反應偵測（multiple reaction monitoring, MRM）模式分析。於15分鐘內同時分析8種植物生長調節劑，分析過程每分鐘流速0.3 mL/min。本分析方法檢量線迴歸決定係數（R^2值）均可達0.997以上，針對常見不同劑型之植物生長調節劑進行回收率試驗，高濃度（0.4 μg/mL）回收率為79.2～121%，低濃度（0.05 μg/mL）回收率為76.5～122%。精密性配製標準液0.1 μg/mL，重複注入分析6次求其相對標準偏差為2.39～3.46%。巴克素等8種植物生長調節劑方法定量極限為0.001%，達法規檢測極限。利用本方法檢測市售6件植物生長調節劑成品農藥，巴克素等8種成分之含量均低於法規檢測極限。相較於現行分析成品農藥中摻雜植物生長調節劑之方法，須以氣相或液相層析質譜儀定性，再分別以各農藥有效成分公告檢驗方法定量；本方法以液相層析串聯質譜儀同時進行8種成分之定性定量，能有效節省人力、時間及溶劑成本。

關鍵字

植物生長調節劑；多重分析方法；液相層析串聯質譜儀

並列摘要

Plant growth regulators (PGR) are plant hormones composed of natural or synthetic substances that can regulate the growth and development of plants. According to Subparagraph 2, Article 7, of Pesticide Management Law as well as Schedule 6, Article 3, of the Pesticide Standard Specification Guidelines, Taiwan, the pesticide tolerance for doping with the active ingredients paclobutrazol, 2- (1-naphthyl) acetamide, uniconazole-P, 4-chlorophenoxyacetic acid (4-CPA), kinetin, forchlorfenuron, and fluroxypyr-meptyl in pesticides is 0.01%, the pesticide tolerance for doping with quinclorac is 3% or 0.1%, depending on different formulation type, and the limit of quantification for doping with the 8 PGRs is 0.001%. As stipulated by the Council of Agriculture, Taiwan, the current method of analyzing these 8 PGRs doped in a formulated agro-pesticide product first requires qualifying them individually by GC-MS or LC-MS, then quantifying each according to specific inspection methods, in which the analysis times are different for each sample. Therefore, the current method is time consuming with high labor and reagent costs. In this study, a multiple analysis method was developed to simultaneously analyze the 8 PGRs. The sample extraction procedure included weighing the sample in a volumetric flask, adding methanol, ultrasonic vibration and making up the solution to a specific volume with methanol. Following filtration, the test liquid was analyzed by liquid chromatography-tandem mass spectrometer(LC-MS/MS) in MRM mode with a flow rate of 0.3 mL/min. This method could simultaneously analyze the 8 PGRs in just 15 minutes. The coefficient of determination of the calibration curves for the 8 PGRs could reach over 0.997. A recovery test against common formulation types revealed that high (0.4 μg/mL) and low (0.05 μg/mL) concentration recovery respectively reached between 79.2% to 121% and 76.5% to 122%. Precision testing was also performed by repeatedly injecting a mixture of the 8 PGRs at 0.1 μg/mL each into the LC-MS/MS six times. The relative standard deviations were approximately 2.39 to 3.46%, and the limit of quantification of the PGRs achieved 0.001%. Furthermore, the analysis results for 6 PGR samples were all below the limit of quantification using this method. Thus, our method using LC-MS/MS is superior to the current method as qualifying as well as quantifying samples can be simultaneously performed with high accuracy and precision, which also effectively reduces labor time and costs, especially costs for solvents.

並列關鍵字

plant growth regulators ； multiple analysis method ； LC-MS/MS

國際替代計量

成品農藥中植物生長調節劑多重檢測分析方法之建立

全文下載

主題瀏覽