SPME-GC/MS method development for synthetic leather worker urinary metabolites

• Main Authors: Chen Szu-Yu, 陳思瑜
• Other Authors: Wang Ven-Shin
• Format: Others
• Language: zh-TW
• Published: 2004
• Online Access: http://ndltd.ncl.edu.tw/handle/70984593558920034470

碩士 === 中國醫藥大學 === 環境醫學研究所 === 92 === SPME-GC/MS method development for synthetic leather worker urinary metabolites Objective：N,N-dimethylformamide (DMF) has been used as a solvent in many industries, especially in artificial leather industry. Urinary N,N-methylformamide (U-NMF) is commonly used as the biomarker of DMF exposure. The purpose of this study is to develop an analytical method for determining the DMF metabolism using solid phase microextraction followed by gas chromatography/mass spectrometry analysis. Method：The Carbowax-Divinylbenzene(CW/DVB) fiber was tested to be the most suitable material for sample extraction. Due to the characteristic of low vaporization of DMF metabolism, and to increasing the DMF metabolism consistency, heating procedure was executed prior to the analysis. The pretreated procedure was then used to extract DMF metabolism in urine by headspace extraction. The SPME fiber was inserted into the injection port of GC/MS and analyzed. The standard solution was prepared by spiking DMF metabolism standard into the blank pooled urine of unexposed person. The optimum extraction parameters investigated were: pH, salt (NaCl, KNO3, NaNO3, (NH4)2SO4), temperature, stirring speed, extraction time, as well as measurement condition of GC/MS. Results： 1.The SPME method was placing 0.8 g NaCl and 4mL urine sample of pH=7±0.2 in an 15mL vial, stirring at 1000 rpm 60 ℃stirring plant, CW/DVB fiber was used to perform headspace solid-phase microextraction for 25 min and thermal desorption 240 ℃for 8 min. 2. For the quality control calibration, the concentration ranges of Acetone, DMF and NMF in urine were 0.1582-31.64 µg/mL, 0.944-188.8 µg/mL, and 1.992-398.4 µg/mL. The correlation coefficients(r) were all above 0.995. The method detection limit（MDL）for Acetone, DMF and NMF were 0.0177 µg/mL, 0.432 µg/mL and 0.446 µg/mL, respectively. 3. In the storage stability tests at -20 ℃, we found the recovery rates for the urine spiked with Acetone at 15.82、0.791 µg/mL, with DMF at 94.4、4.72 µg/mL, and with NMF at 199.2、9.96 µg/mL were all above 86 % within 4 weeks. Conclusion：The analytical method of DMF metabolism by HS-SPME-GC-MS can be reduced complicated pretreated procedure, as well as having the advantage of solvent-free, rapidity, simplicity, and avoid interfering with a complex matrix. Key word：N,N-dimethylformamide, biomarker, solid phase microextraction, headspace