線上固相萃取連結液相層析質譜儀分析牛乳中愛比菌素與伊維菌素殘留

Analysis of Abamectin and Ivermectin Residue in Milk by Online Solid-Phase Extraction Coupled to Liquid Chromatography-Mass Spectrometry

劉亮君(Liang-Chun Liu)

指導教授 ： 鄭建業

中原大學/理學院/化學研究所/碩士(2013年)

https://doi.org/10.6840/CYCU.2013.00363

摘要

愛比菌素(Abamectin)為一種除草劑，其藥性對人體危害甚大，牛群在食用加了此種除草劑的草料後，造成體內殘留，進一步危害人體的健康；而伊維菌素(Ivermectin)則為殺蟲劑，施打於牛隻後造成殘留，亦會間接危害人體的安全，因此必須建立精確、準確及快速有效率的檢驗方法，對此二種藥物殘留進行檢測，以避免此二種藥物殘留的發生。
本研究發展管柱轉換技術線上結合固相萃取裝置與液相層析電噴灑離子化離子阱串聯質譜儀，進行牛奶樣品的線上基質去除，來檢測牛奶中愛比菌素與伊維菌素之殘留，並與紫外光偵測器做比較。離子阱質譜儀的偵測使用正離子多重反應二次質譜監偵測模式。兩種藥物二次質譜之基質強化外標準品檢量線，於濃度範圍0-15 ng/mL具良好線性(愛比菌素之R2 = 0.9938，伊維菌素之R2 = 0.9990)，偵測極限值與定量極限值可達0.67 ng/mL及2.23 ng/mL (愛比菌素)與0.63 ng/mL及2.11 ng/mL (伊維菌素)。
以標準品添加測試五種市售品牌牛奶樣品，發現兩種品牌牛奶均具有接近偵測極限值的微量愛比菌素(0.65 及0.57 ng/mL)及伊維菌素(0.79 及1.04 ng/mL)，另三種品牌牛奶樣品中之愛比菌素及伊維菌素含量，則遠低於偵測極限值並接近0 ng/mL。總而言之，五種品牌牛奶之愛比菌素及伊維菌素均低於法規10 ppb之最大容許殘留量。兩種品牌牛奶分析之準確度為84 %與82 %(愛比菌素)及82 %與88%(伊維菌素)，精密度為8.0% 與7.3% (愛比菌素)及4.8 % 與9.7 % (伊維菌素)。樣品分析一次的時間為10分鐘。整體而言，所發展之方法具有快速，良好的靈敏度、精密性及準確性，並成功的應用在牛奶中愛比菌素與伊維菌素的殘留分析。

關鍵字

液相層析電噴灑離子化離子阱串聯質譜儀 ； 牛奶 ； 愛比菌素 ； 伊維菌素 ； 固相萃取

並列摘要

Abamectin (ABA) is a kind of herbicide and is seriously harmful to human health. After feeding the cattle by abamectin added forage, abamectin residues will remain in the body, which will further endanger the health of human. Ivermectin are antiparasitic agents. Treat the cattle with Ivermectin will also cause residue that indirectly endangers the safety of human. Therefore, a fast, precise, accurate, and efficient method for monitoring the two kinds of residues must be established to avoid their occurrence.
In this study, on-line coupling of a solid-phase extraction column to the liquid chromatography electrospray ionization ion-trap tandem mass spectrometer was developed by the column-switching technique to perform the on-line matrix reduction of milk samples and the inspection of Abamectin and Ivermectin residues in milk. The results will be compared with UV dection. The detection of the ion-trap mass spectrometer uses multiple-reaction monitoring secondary mass spectrometry in positive ion mode. The concentration range of the matrix-enhanced external standard calibration curve of the secondary mass spectrometry for the two kinds of drug was 0-15 ng/mL which exhibits very good linearity with R2 equaling to 0.9938 (Abamectin) and 0.9990 (Ivermectin). The limit of detection (LOD) and quantification (LOQ) were 0.67 ng/mL and 2.23 ng/mL for Abamection, respectively, and 0.63 ng/mL and 2.11 ng/mL for Ivermectin, respectively.
Quantification of Abamectin and Ivermectin in milk samples of five different brands by the standard addition method indicates that two brands of milk samples contain trace amounts of Abamectin (0.65 and 0.57 ng/mL) and Ivermectin (0.79 and 1.04 ng/mL), both of which close to the detection limit. Abamectin and Ivermectin in the milk samples of the other three brands are all well below the LOD and close to zero ng/mL. Overall, the content of Abamectin and Ivermectin in the five brands of milk are all lower than the requlated maximum residue limit (10 ppb). The analytical accuracy of the the two brands of milk samples was 84% and 82% for Abamectin, respectively, and 82% and 88% for Ivermectin, respectively; the precisions were 8.0% and 7.3% for Abamectin, respectively, and 4.8% and 9.7% for Ivermectin, respectively. The analysis time for one sample was 10 min. Overall, the developed method is fast, sensitive, precise, and accurate and is successfully applied for the Abamectin and Ivermectin residue analysis of milk samples.

並列關鍵字

milk. ； Solid-phase extraction ； Liquid chromatography -electrospray ionization ion-trap tandem mass spectrometry ； Abemectin ； Ivermectin

參考文獻

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