职业接触丙酮生物标志物—尿中丙酮的标准检测方法研制

发布时间：2018-05-06 09:44

  本文选题：尿丙酮 + 生物监测　； 参考：《武汉科技大学》2012年硕士论文

【摘要】：目的 丙酮是实验室和工业上广泛使用的有机溶剂，，对其进行环境监测和生物监测意义重大。职业接触丙酮的生物标志物主要有尿丙酮、血丙酮及肺泡气丙酮，研究表明尿中丙酮浓度与丙酮接触人群的环境暴露浓度相关性最高，是丙酮生物监测的最佳生物标志物。美国ACGIH和德国DFG都已将尿丙酮作为接触者的生物监测指标，并制定了相关卫生标准，分别规定其生物接触限值为50mg/l(BEI)和80mg/l（BAT）。我国在这方面的研究尚属起步阶段，本课题欲研制职业接触丙酮的生物标志物尿丙酮的标准检测方法，为我国丙酮职业暴露的生物监测方法提供标准依据，为下一步尿丙酮生物接触限值的制定提供技术支持。 方法 采用顶空技术对尿丙酮进行气相萃取分离，以减小尿液基底对分析测定的干扰，提高检测方法灵敏度，同时用气相色谱仪和FID检测器对分离后的气态丙酮进行定性定量分析。通过对顶空参数和色谱参数指标的最优试验选择，研制符合我国职业卫生标准制定指南要求的尿丙酮顶空—气相色谱标准检测方法，并对方法的检出限、准确度、精密度、样品存放稳定性、抗干扰性以及现场应用能力等性能指标进行测试评价。 结果 在20ml的顶空瓶中，当取尿液体积3ml,加入无水硫酸钠盐4g，在50℃恒温水浴锅中水浴20min时，样品预处理效果最佳，尿丙酮的顶空—气相色谱法检测灵敏度最高。本研制方法在4.9～157.6mg/L的检测范围内，有较好线性，线性回归方程为Y＝3196.3X+4753（r=0.9995），由标准差法测得的检出限为0.67mg/L。准确度用加标回收试验测试，低、中、高三个浓度的平均加标回收率分别为93．92%、104．46％和101.20%，日内与日间精密度以相对标准偏差（RSD）表示，其范围分别为5.69%～9.33%和6.44%～9.34%。环境中共存的甲醇、二氯甲烷、丁酮等物质不干扰尿中丙酮的测定。该方法的稳定性实验表明，在4℃保存时，样品稳定性最好，可存放至少一周。 结论 本研究研制的尿丙酮顶空—气相色谱测定方法具有操作简单、准确度高、干扰少等优点，能满足职业卫生标准制定指南对生物材料测定方法各指标的性能要求，可推荐作为我国职业接触丙酮生物标志物尿中丙酮的生物监测标准方法。若要进一步提高方法的精密度，可采用自动顶空进样装置，方法的稳定性会更好。
[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

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