以高效液相層析法同時分析飼料和肉品中磺胺劑與四環素   全文下載

Simultaneous Determination of Sulfa Drugs and Tetracyclines in Feeds and Animal Tissues by High-Performance Liquid Chromatography

本研究係對國內常用家畜飼料所添加之六種磺胺劑、三種四環素類抗生素和化學療法劑卡巴得及其在屠體肉品及內臟中之殘留量以高效液相層析法找出四種最佳分析條件：一、用LiChrosorb RP-C18分離管，以5%氰甲烷混水溶液加0.1M磷酸緩衝液（pH 7.4）為移動相，於UV 254nm檢測之可同時分析SDA，SMM，STA，SDM，SMT和SQO。二、用Ultrasphere ODS分離管，以含15%氰甲烷之0.1 M磷酸緩衝液（pH 6.8）為移動相，於UV 254nm檢測之可同時分析SDA，SMM，STA，SMT，SQO及SDM。三、用LiChrosorb RP-C18分離管，以7%異丙醇水溶液內含0.001M Na2EDTA和0.1 M二乙醇胺緩衝液（pH 7.3）為移動相，於UV 254nm檢測之可同時分析STA，SMT、卡巴得，TC，OTC及CTC。四、用Alltech RP-C18分離管，以28%二甲基甲胺水溶液內含0.001M Na2EDTA，0.05M檸檬酸，0.013M檸橡酸鈉和0..1M KNO3緩衝液（pH 3.0）為移動相，於UV 280nm檢測之可同時分析STA，SMT，OTC，卡巴得及CTC。飼料添加藥物回收率介於85-99%之間；肉品及內臟中回收率亦達69-80%。總共有廿種市售飼料檢樣中，十一種飼料樣品被檢出含有禁用磺胺劑或四環素類抗生素。廿一種肉品及內臟檢樣中，一種豬肉檢樣OTC殘留量和二種豬肝檢樣總磺胺劑殘留量皆超過法定容許量。飼料中藥物檢出最低限量為1.0-5.0 ppb；肉品及內臟藥物殘留量檢出最低限量為2.0-12 ppb。

This study aimed to develop a high-performance liquid chromatographic method for simultaneous determination of six sulfa drugs, three tetracycline antibiotics and carbadox in feeds and animal tissues. Four successful conditions were established : 1. On LiChrosorb RP-C18 column with water: acetonitrile (95:5, v/v) as mobile phase and UV detector at 254nm to separate SDA, SMM, STA, SDM, SMT and SQO. 2. On Ultrasphere ODS Column with water: acetonitrile (85:15, v/v) as mobile phase and detected at UV 254nm to separate SDA SMM. STA SMT, SQO and SDM. 3. On LiChrosorb RP-C18 column with water: isopropanol (93:7, v/v) as mobile phase and detected at UV 254nm to separate STA, SMT, Carbadox, TC, OTC and CTC. 4. On Alltech RP-C18 column with water: dimethylformamide (72:28, v/v) as mobile phase and detected at UV 280nm to separate STA SMT, OTC, Carbadox and CTC. The recoveries of the drugs in feeds were between 85-99%; in animal tissues, 69-80%. Eleven out of 20 feed samples were found with prohibited sulfa drugs or tetracyclines added. One pork sample with OTC residue and two pig liver samples with total sulfa drugs residue exceeding the maximum tolerance limits wee detected from the 21 meat samples analyzed. The lowest detection limits of residual drugs were between 1.0-5.0 ppb in feeds; 2.0-12 ppb in animal tissues.