七种常见巴比妥和导眠能的气液色谱法及其从脏器肝和尿中的检出

GAS-LIQUID CHROMATOGRAPHIC ISOLATION AND IDENTIFICATION OF SEVEN BARBITURATES AND GLUTETHIMIDE FROM LIVER AND URINE

本文用浓度1.5％的OV-17和SE-52填充柱研究了巴比妥、异戊巴比妥、戊巴比妥、速可眠、硫喷妥、苯巴比妥、美导眠(Heptabarbitone)等七种常见巴比妥和导眠能的气液色谱分离检定条件并实际应用于从人尿,人肝、狗肝、兔肝中检出某些巴比妥类药物。同分异构体如异戊巴比妥和戊巴比妥用本法可以得到较明显的分离。一次色谱过程最多只要20分钟,故为一个快速、高效、灵敏的方法。

GLC of barbitone, amytal, pentobarbital, secobarbital, thiobarbitone, heptabarbitone and glutethimide is reported by using glass column packed with 1.5% SE-52 on chromosorb W (60～80 mesh)and stainless steel column packed with 1.5% OV-17 on shimalite W (80～100 mesh). The gas chromatograph is equipped with FID using N_2 as the carrier gas, at a flow of 25 ml per minute (SE-52) and 50 ml per minute (OV-17). The column is maintained at 200℃ and the injection port and the detector at 250℃. The method is successfully applied to the isolation and identification of some barbiturates from urine and liver of human, dog or rabbit.Extraction procedure: Triturate 5 g of liver in a conical flask and add 0.3 ml of 6N HCl, 50 ml of ether. Shake vigorously and pour the organic phase into the refining column(containing 2 g of active charcoal, 20 g of aluminium oxide for chromatography and 20 g of anhydrous sodium sulfate). Gollect the eluate into a separator and extract with 0.45 N NaOH. Acidify the alkaline extract by 6 N HCl, then extract successively with 20 ml and 15 ml of ether. Deaquate the combined ether solution by anhydrous sodium sulfate. Evaporate the ether and dissolve the residue in 0.5 ml of methylene chloride. Inject 0.6～1.0 μl of this solution into gas chromatograph.