頂空-固相微萃取-氣相色譜法測定尿中丁酮
發(fā)布時間:2018-01-19 08:03
本文關鍵詞: 頂空固相微萃取 氣相色譜 丁酮 尿 出處:《現(xiàn)代預防醫(yī)學》2017年04期 論文類型:期刊論文
【摘要】:目的建立頂空-固相微萃取-氣相色譜法測定尿中丁酮的方法。方法利用頂空技術,將適量鹽析劑和待測丁酮溶液置于20 ml頂空瓶中,混合均勻后置于一定溫度的水浴鍋中,經DVB/CAR/PDMS固相微萃取萃取頭吸附頂空氣中的丁酮,待平衡后將纖維頭取出、插入氣相色譜氣化室,熱解吸涂層上吸附的丁酮,經毛細管色譜柱分離,FID檢測器檢測。結果 DVB/CAR/PDMS萃取頭、20 min萃取時間、30℃平衡溫度、2.0g Na Cl鹽析條件下,丁酮的測定范圍為0.5~5.0μg/ml,相關系數(shù)r=0.9999,方法檢出限為0.005μg/ml,精密度0.72%~4.63%,方法回收率94.7%~101.2%。結論該方法各指標滿足我國生物材料中化學物質測定方法的要求,適用于職業(yè)接觸丁酮勞動者尿中丁酮的檢測。
[Abstract]:Objective to establish a method for the determination of butanone in urine by headspace solid phase microextraction gas chromatography. Methods proper amount of salting-out agent and butanone solution were placed in 20ml headspace bottle by headspace technique. The mixture was evenly mixed and placed in a water bath at a certain temperature. The butanone in the top air was adsorbed by the DVB/CAR/PDMS solid-phase microextraction head. The fiber head was removed after equilibrium and inserted into the gas chromatographic gasification chamber. Butanone adsorbed on the thermal desorption coating was determined by capillary column separation and FID detector. Results the extraction time of DVB/CAR/PDMS extractor was 20 min and the equilibrium temperature was 30 鈩,
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