QuEChERS-超高效液相色譜-串聯質譜法測定畜肉中伊維菌素殘留量

金鑫 朱志

摘 ?要：采用QuEChERS技術提取畜肉中的伊維菌素（ivermectin，IVM），經堿性氧化鋁固相萃取柱凈化后氮吹濃縮，以乙腈和2.5 mmol/L乙酸銨水溶液為流動相，經Kinetex C18色譜柱洗脫分離，采用電噴霧離子源，多反應監測正離子模式進行分析，建立超高效液相色譜-三重四極桿串聯質譜法測定畜肉中IVM含量的分析方法。結果表明：在1.0～500.0 μg/kg添加量范圍內，IVM質譜響應強度與其質量濃度呈良好的線性關系，相關系數（r）為0.999 7;檢出限為0.3 μg/kg，定量限為1.0 μg/kg;加標回收率為94.7%～97.4%，相對標準偏差為1.0%～3.2%。該法前處理簡單、準確度高、精密度好，可為畜牧養殖和畜肉質量安全監控提供檢測方法。

關鍵詞：伊維菌素;超高效液相色譜-串聯質譜法;QuEChERS;畜肉;殘留量測定

Abstract： This paper reports on the development of an analytical method for the determination of ivermectin residues in livestock meat using ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry （UPLC-MS/MS）. Ivermectin from samples was extracted by the QuEChERS method， purified by solid phase extraction on an alkaline alumina column and concentrated by nitrogen blowing. Using a mobile phase consisting of acetonitrile and 2.5 mmol/L ammonium acetate aqueous solution， the chromatographic separation was performed on a Kinetex C18 column. The analyte was detected by multiple reaction monitoring （MRM） with an electrospray ionization source in the positive ion mode. The results showed that the concentration of ivermectin in the range from 1.0 to 500.0 μg/kg showed a good linear relationship with mass spectral response values， with a correlation coefficient （r） of 0.9997. The limit of detection and limit of quantitation were 0.3 and 1.0 μg/kg， respectively. The recoveries for spiked samples were in the range from 94.8% to 97.4%， with relative standard deviations （RSDs） of 1.3% to 3.2%. The method had the advantages of simple pretreatment， high accuracy and good recovery， and it could be useful in animal husbandry and livestock meat quality and safety supervision.

Keywords： ivermectin; ultra-high performance liquid chromatography-tandem mass spectrometry; QuEChERS; livestock meat; residue determination

DOI：10.7506/rlyj1001-8123-20190802-174

中圖分類號：TS251.7 ? ? ? ? ? ? ? ? ? 文獻標志碼：A ? ? ? ? ? ? ?文章編號：

伊維菌素（ivermectin，IVM），又名22，23-二氫阿巴美丁或依維菌素[1-2]，化學式為C48H74O14，是由鏈霉菌（Streptomyces avermitilis）發酵產生的十六元大環內酯化合物[3-5]，對體內外寄生蟲，特別是線蟲和節肢動物具有良好的驅殺功效，是一種高效、廣譜、低毒抗生素類抗寄生蟲藥物[6-8]，廣泛用于治療家畜的胃腸線蟲病、牛皮蠅蛆、紋皮蠅蛆、羊鼻蠅蛆和豬、羊疥螨病[9-11]。我國農業部規定IVM在牛腎臟組織中的最高殘留限量（maximum residue limit，MRL）為30 μg/kg;歐盟（EU）No418/2014號法規規定IVM在動物源性食品中的MRL為30～100 μg/kg;日本“食品中殘留農業化學品肯定列表制度”規定IVM在牛、豬、馬、羊等畜肉中的MRL為10～100 μg/kg[6-7，9]。但IVM會通過動物飼料中添加、動物寄生蟲預防和治療等途徑導致家畜體內IVM殘留，經食物鏈進入人體，若長期誤食含有IVM殘留的家畜肉，將導致人體神經系統及生殖系統紊亂[12-14]，甚至威脅人類健康。……