以高效液相層析檢測水果中三亞蟎殘留量   全文下載

The Relationship between the Cold Chain System and Vaccine Potency in Taiwan: (I) Live Measles Vaccine and MMR Vaccine

本研究發展出以高效液相層析法檢驗水果中三亞?殘留量之方法。稱取20g檢體及2g碳酸氫鈉，以丙酮均質抽取，抽取液抽氣過濾後加入1g氯化鈉，以正己烷乙酸乙酯（8:2, v／v）溶液萃取，有機溶媒層或壓濃縮至5mL後注入矽酸鎂固相萃取匣，以10mL正己烷：乙酸乙酯（8:2, v／v）溶液沖提，沖提液減壓濃縮至乾以乙?定容並以HPLC附UV檢出器分析。層析管為Lichrosorb RP-18，移動相為乙?：水（80:20, v／v），UV檢出器設定為313 nm。添加三亞?於蘋果中，檢體濃度為0.25～0.75 ppm，所得平均回收率為88.8～92.1%；添加於葡萄柚中，檢體濃度為0.1～0.3 ppm，所得平均回收率為87.2～90.9%。本檢驗方法之最低檢出限量為0.02 ppm。"

A high performance liquid chromatographic method (HPLC) for the determination of amitraz residue in fruits has been developed. Twenty grams of sample and 2 g of sodium hydrogen carbonate were weighed and homogenized with acetone. After vacuum filtration, 1 g NaCl was added and partitioned with n-hexane containing 20% ethyl acetate. The organic layer was evaporated to 5 mL and applied on a florisil cartridge. The cartridge was eluted with 10 mL n-hexane:ethyl acetate (8:2, v/v), and the eluate was evaporated to dryness. The residue was dissolved in acetonitrile and determined by HPLC equipped with a UV detector. Separation was conducted with a Lichrosorb RP-18 column using acetonitrile: H2O (80:20, v/v) as mobile phase to separate amitraz and interferences, and amitraz was determined at 313 nm wavelength. Recovery studies were carried out by spiking the amitraz standards to the levels of 0.25~0.75 ppm in apples and 0.1~0.3 ppm in grapefruit. The average recoveries were 88.8~92.1% and 87.2~90.9% for apples and grapefruit, respectively. The detection limit was 0.02 ppm. 本研究發展出以高效液相層析法檢驗水果中三亞蟎殘留量之方法。稱取20g檢體及2g碳酸氫鈉，以丙酮均質抽取，抽取液抽氣過濾後加入1g氯化鈉，以正己烷乙酸乙酯（8:2, v／v）溶液萃取，有機溶媒層或壓濃縮至5mL後注入矽酸鎂固相萃取匣，以10mL正己烷：乙酸乙酯（8:2, v／v）溶液沖提，沖提液減壓濃縮至乾以乙腈定容並以HPLC附UV檢出器分析。層析管為Lichrosorb RP-18，移動相為乙腈：水（80:20, v／v），UV檢出器設定為313 nm。添加三亞蟎於蘋果中，檢體濃度為0.25～0.75 ppm，所得平均回收率為88.8～92.1%；添加於葡萄柚中，檢體濃度為0.1～0.3 ppm，所得平均回收率為87.2～90.9%。本檢驗方法之最低檢出限量為0.02 ppm。