本文選題：尿丙酮 + 生物監(jiān)測　； 參考：《武漢科技大學(xué)》2012年碩士論文

【摘要】：目的 丙酮是實驗室和工業(yè)上廣泛使用的有機溶劑，，對其進行環(huán)境監(jiān)測和生物監(jiān)測意義重大。職業(yè)接觸丙酮的生物標志物主要有尿丙酮、血丙酮及肺泡氣丙酮，研究表明尿中丙酮濃度與丙酮接觸人群的環(huán)境暴露濃度相關(guān)性最高，是丙酮生物監(jiān)測的最佳生物標志物。美國ACGIH和德國DFG都已將尿丙酮作為接觸者的生物監(jiān)測指標，并制定了相關(guān)衛(wèi)生標準，分別規(guī)定其生物接觸限值為50mg/l(BEI)和80mg/l（BAT）。我國在這方面的研究尚屬起步階段，本課題欲研制職業(yè)接觸丙酮的生物標志物尿丙酮的標準檢測方法，為我國丙酮職業(yè)暴露的生物監(jiān)測方法提供標準依據(jù)，為下一步尿丙酮生物接觸限值的制定提供技術(shù)支持。 方法 采用頂空技術(shù)對尿丙酮進行氣相萃取分離，以減小尿液基底對分析測定的干擾，提高檢測方法靈敏度，同時用氣相色譜儀和FID檢測器對分離后的氣態(tài)丙酮進行定性定量分析。通過對頂空參數(shù)和色譜參數(shù)指標的最優(yōu)試驗選擇，研制符合我國職業(yè)衛(wèi)生標準制定指南要求的尿丙酮頂空—氣相色譜標準檢測方法，并對方法的檢出限、準確度、精密度、樣品存放穩(wěn)定性、抗干擾性以及現(xiàn)場應(yīng)用能力等性能指標進行測試評價。 結(jié)果 在20ml的頂空瓶中，當(dāng)取尿液體積3ml,加入無水硫酸鈉鹽4g，在50℃恒溫水浴鍋中水浴20min時，樣品預(yù)處理效果最佳，尿丙酮的頂空—氣相色譜法檢測靈敏度最高。本研制方法在4.9～157.6mg/L的檢測范圍內(nèi)，有較好線性，線性回歸方程為Y＝3196.3X+4753（r=0.9995），由標準差法測得的檢出限為0.67mg/L。準確度用加標回收試驗測試，低、中、高三個濃度的平均加標回收率分別為93．92%、104．46％和101.20%，日內(nèi)與日間精密度以相對標準偏差（RSD）表示，其范圍分別為5.69%～9.33%和6.44%～9.34%。環(huán)境中共存的甲醇、二氯甲烷、丁酮等物質(zhì)不干擾尿中丙酮的測定。該方法的穩(wěn)定性實驗表明，在4℃保存時，樣品穩(wěn)定性最好，可存放至少一周。 結(jié)論 本研究研制的尿丙酮頂空—氣相色譜測定方法具有操作簡單、準確度高、干擾少等優(yōu)點，能滿足職業(yè)衛(wèi)生標準制定指南對生物材料測定方法各指標的性能要求，可推薦作為我國職業(yè)接觸丙酮生物標志物尿中丙酮的生物監(jiān)測標準方法。若要進一步提高方法的精密度，可采用自動頂空進樣裝置，方法的穩(wěn)定性會更好。
[Abstract]:Purpose Acetone is a widely used organic solvent in laboratory and industry. The main biomarkers of occupational exposure to acetone were urine acetone, blood acetone and alveolar acetone. Both ACGIH and DFG of Germany have used urinary acetone as a biological monitoring index for exposed people and have established relevant hygienic standards, which stipulate the biological exposure limits of 50 mg / L BEI and 80 mg / L BATI, respectively. The research in this field is still at the initial stage in our country. This project is to develop the standard detection method of urinary acetone, which is a biomarker of occupational exposure to acetone, and provide the standard basis for the biological monitoring method of occupational exposure to acetone in China. To provide technical support for the next step to establish the biological exposure limit of urinary acetone. Method The headspace technique was used to separate urine acetone by gas phase extraction, in order to reduce the interference of urine substrate to the analysis and determination, and to improve the sensitivity of the method. At the same time, the gas chromatograph and FID detector were used to qualitatively and quantitatively analyze the separated gaseous acetone. Based on the optimum selection of headspace parameters and chromatographic parameters, a method for the determination of headspace urine acetone headspace gas chromatography was developed according to the guidelines for occupational health standards in China. The detection limit, accuracy and precision of the method were also studied. Sample storage stability, anti-interference and field application capability were tested and evaluated. Result In the headspace bottle of 20ml, when the urine volume is 3 ml, the anhydrous sodium sulfate is added 4 g, and the water bath 20min is in the constant temperature water bath at 50 鈩

本文編號：1851827