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目的建立顶空-固相微萃取-气相色谱法测定尿中丁酮的方法。方法利用顶空技术,将适量盐析剂和待测丁酮溶液置于20 ml顶空瓶中,混合均匀后置于一定温度的水浴锅中,经DVB/CAR/PDMS固相微萃取萃取头吸附顶空气中的丁酮,待平衡后将纤维头取出、插入气相色谱气化室,热解吸涂层上吸附的丁酮,经毛细管色谱柱分离,FID检测器检测。结果 DVB/CAR/PDMS萃取头、20 min萃取时间、30℃平衡温度、2.0g Na Cl盐析条件下,丁酮的测定范围为0.5~5.0μg/ml,相关系数r=0.9999,方法检出限为0.005μg/ml,精密度0.72%~4.63%,方法回收率94.7%~101.2%。结论该方法各指标满足我国生物材料中化学物质测定方法的要求,适用于职业接触丁酮劳动者尿中丁酮的检测。
Objective To establish a method for the determination of butanone in urine by headspace-solid phase microextraction-gas chromatography. Methods Headspace technology was used. The appropriate amount of salting-out agent and the solution of butanone to be measured were placed in a 20 ml headspace bottle. After mixing, the cells were placed in a water-bath with a certain temperature and subjected to DVB / CAR / PDMS SPE Adsorption of butanone in the top air, to be balanced after the fiber head removed, inserted into the gasification gasification chamber, thermal desorption adsorption of butanone on the coating, the capillary column separation, FID detector detection. Results The calibration curve of butanone with DVB / CAR / PDMS extraction head, extraction time of 20 min, equilibrium temperature of 30 ℃, and salting-out of 2.0 g NaCl was 0.5 ~ 5.0 μg / ml with the correlation coefficient r = 0.9999. Limit of 0.005μg / ml, precision 0.72% ~ 4.63%, the method recovery 94.7% ~ 101.2%. Conclusion The methods meet the requirements of the method for the determination of chemical substances in biomaterials in our country and are suitable for the determination of butanone in the urine of the occupational buttermilk workers.