Ryan J J, Pilon J C
J Assoc Off Anal Chem. 1976 Jul;59(4):817-20.
A simple chemical technique was developed to confirm the presence of diethylstillbestrol (DES) residues in beef tissues at 2 ppb. The DES-trifluoroacetate (TFA) from the previously published method is hydrolyzed in water-methanol at 55 degrees C for 20 min to free DES which is then extracted into benzene. Trimethylamine and a small amount of heptaafluorobutyric (HFB) anhydride are added to effect the smooth conversion of DES to its di-HFB at either room temperature or 60 degrees C. DES-HFB is determined by gas-liquid chromatography with electron capture detection on a 6' x 4 mm id column of 3% OV-210 at 190 degrees C. This procedure yields 2 peaks for DES-HFB (retention times 2.7 and 4.8 min for the cis and trans, respectively) which are resolved from the 2 DES-TFA peaks (retention times 2.3 and 3.3 min for cis and trans, respectively). The sensitivity of detection of DES-HFB is increased by a factor of 4-5 over that for DES-TFA. This chemical technique was successfully applied to purified extracts of beef liver fortified with DES at 2-10 ppb with recoveries from 60 to 110%.
开发了一种简单的化学技术，用于确认牛肉组织中是否存在浓度为2 ppb的己烯雌酚（DES）残留。将先前发表方法中的DES - 三氟乙酸酯（TFA）在55℃的水 - 甲醇中水解20分钟，以释放出DES，然后将其萃取到苯中。加入三甲胺和少量七氟丁酸（HFB）酐，在室温或60℃下使DES顺利转化为其二 - HFB。通过气相色谱 - 电子捕获检测法在190℃下于内径为6'×4 mm的3% OV - 210柱上测定DES - HFB。此方法产生2个DES - HFB峰（顺式和反式的保留时间分别为2.7分钟和4.8分钟），它们与2个DES - TFA峰（顺式和反式的保留时间分别为2.3分钟和3.3分钟）得以分离。DES - HFB的检测灵敏度比DES - TFA提高了4至5倍。该化学技术成功应用于添加了2至10 ppb DES的牛肉肝纯化提取物，回收率为60%至110%。
