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目的建立顶空-固相微萃取-气相色谱法测定尿液中四氢呋喃含量的方法。方法通过顶空-固相微萃取技术使尿样中的四氢呋喃经过水浴加热,挥发吸附于固相微萃取纤维上,气相色谱仪解吸萃取纤维上吸附的四氢呋喃并定量检测。顶空固相微萃取选择DVB/CAR/PDMS萃取纤维效果最佳;水浴条件为40℃,加2.50 g无水硫酸钠平衡10 min;气相色谱仪柱温选择80℃。结果在优化的条件下,尿中四氢呋喃的检出限为0.005 3 mg/L,测定范围为0.22 mg/L~4.45 mg/L,相关系数(r)为0.999 8,加标回收率为91.8%~101.1%,相对标准偏差(RSD)为5.50%~7.24%。结论采用顶空-固相微萃取-气相色谱法测定尿液中四氢呋喃,简便快速、检出限低、结果准确可靠,可用于职业接触四氢呋喃人群尿中四氢呋喃的测定。
Objective To establish a method for the determination of tetrahydrofuran in urine by headspace-solid phase microextraction-gas chromatography. Methods The headspace-solid phase microextraction technique was used to make tetrahydrofuran in urine samples heated in a water bath, volatilized and adsorbed onto SPME fibers. The THF adsorbed on the fibers was desorbed and quantified by gas chromatography. Headspace solid-phase microextraction selected DVB / CAR / PDMS fiber extraction best; water bath conditions were 40 ℃, add 2.50 g anhydrous sodium sulfate balance 10 min; gas chromatograph column temperature 80 ℃. Results Under the optimal conditions, the detection limit of tetrahydrofuran in urine was 0.005 3 mg / L, the determination range was 0.22 mg / L ~ 4.45 mg / L, the correlation coefficient was 0.999 8, the recoveries were 91.8% ~ 101.1%, the relative standard deviation (RSD) was 5.50% ~ 7.24%. Conclusion The determination of tetrahydrofuran in urine by headspace-solid phase microextraction-gas chromatography has the advantages of simple and rapid detection, low detection limit, and accurate and reliable determination of tetrahydrofuran in urine of occupational exposure to tetrahydrofuran.