高通量全自动检测技术在空气中甲醛含量测定的应用研究

Application of high-throughput fully automated air formaldehyde detection technology

[背景]甲醛是一种有毒有害的气体,全自动碘分析仪是一种测量水碘、尿碘的高通量全自动检测仪器,目前,其在空气中甲醛含量测定的应用研究尚未见报道。[目的]建立一种基于全自动碘分析仪的空气中甲醛含量测定的高通量检测方法。[方法]空气中甲醛经采样器采集,移取1.0 mL工作曲线溶液、标准物质溶液以及样品溶液,上机,一键启动,全自动碘分析仪进行全自动测量结果计算。分别对溶液静置时长和仪器工作参数[检测波长,样品针下降深度和试剂2(R_(2))反应时间]进行优化;最后进行方法学验证,其中包括精密度、检出限、定量限和加标回收实验;用4种不同浓度的标准物质样品溶液以及采集的10份空气样品进行手工法与高通量全自动检测两种方法做平行比较应用考察。[结果]本研究最终优化的条件为:配制好的溶液静置2 h及以上;仪器工作最优参数为:检测波长660 nm,样品针下降深度2800,R2反应时间为900 s。方法学验证,线性关系为光密度(D)=0.9787×甲醛溶液浓度(C)0.0364,相关系数为1.0000,检出限和定量限分别是0.015、0.052μg·mL^(-1),两个不同浓度的标准物质样品溶液日内精密度实验的相对标准偏差(RSD)分别是1.35%和1.18%,日间精密度实验的RSD分别为1.82%和1.50%。回收率实验测得的回收率在96.8%~107.4%。4种不同浓度的标准物质样品溶液以及采集的10份空气样品进行可见分光光度计与全自动碘分析仪两种测量方法的平行比较应用考察,两种方法检测结果相近,4种不同浓度的标准物质样品溶液测量结果均在不确定度范围内。[结论]本研究建立的空气中甲醛含量测定在全自动碘分析仪的检测方法,具有溶剂用量小,全自动高通量等特点,具有与国标相当的方法灵敏度,准确度高,日间日内精密度良好,回收率在96%以上,可为空气中甲醛含量测定提供有力的技术支持。

[Background]Formaldehyde is a toxic gas.Automatic iodine analyzer is a high-throughput automatic instrument for measuring water and urine iodine,but at present,there is a lack of its application in the determination for air formaldehyde.[Objective]To develop a high-throughput method for air formaldehyde determination with an automated iodine analyzer.[Methods]The formaldehyde in the air was collected with an atmospheric sampler,and 1.0 mL of working curve solution,standard solution,and sample solution were loaded to an automated iodine analyzer.Solution resting time and instrumental parameters,including detection wavelength,sample needle depth,and regent_(2)(R_(2))reaction time were optimized.Finally,the method was validated by precision,detection and quantification limits,and spiked recovery.Four different concentrations of standard substance solutions and 10 air samples were collected for comparison between manual measurement method and high-throughput fully automated detection method.[Results]The final optimized conditions in this study were:2 h and above resting time for prepared solution,and the optimal parameters of the instrument work were:detection wavelength at 660 nm,sample needle depth at 2800,and R2 reaction time at 900 s.Under the optimized conditions the linear equation of the method was optical density(D)=0.9787×formaldehyde concentration(C)−0.0364 and the correlation coefficient was 1.0000.The limits of detection(LOD)and quantification(LOQ)were 0.015μg·mL^(−1) and 0.052μg·mL^(−1),respectively.The relative standard deviations(RSDs)of the intra-day precision experiments were 1.35%and 1.18%for the two different concentrations of standard sample solutions.The RSDs of the inter-day precision experiments were 1.82%and 1.50%,respectively.The recoveries ranged from 96.8%to 107.4%.The results produced by spectrophotometry and automated detection method in the comparison study were identical,and the measurements of selected four concentrations of standard solutions were within the uncertainty range.[Conclusion]The method established in this study features small solvent dosage,fully automated high throughput,comparable sensitivity to the national standard method,high accuracy,and inter-day and intra-day precision with a recovery rate above 96%.It can provide strong technical support for the determination of air formaldehyde.