人体血尿中挥发性有机物检测方法建立及应用

发布时间：2018-01-08 20:17

本文关键词：人体血尿中挥发性有机物检测方法建立及应用　出处：《中国疾病预防控制中心》2017年硕士论文　论文类型：学位论文

【摘要】：为掌握我国重点地区主要环境污染对人群健康影响的基本状况,评估环境污染带来的健康风险,环保部会同国家卫计委于2015-2017年联合组织开展“全国重点地区环境与健康专项调查”(以下简称“专项调查”)。本研究作为专项调查的一部分,主要负责建立血中挥发性有机物检测方法和实验室质量控制相关工作。目的建立血、尿中13种挥发性有机物(VOCs)的检测方法。方法以吹扫捕集-气质联用和固相微萃取-气质联用为实验平台,使用消泡剂和同位素内标,在高纯氮气环境下处理样品,采用“倍比稀释法”建立校准曲线,建立了吹扫捕集-气相色谱/质谱-同位素内标法检测全血/尿中挥发性有机物、固相微萃取-气相色谱/质谱-同位素内标法检测全血中挥发性有机物三种检测方法。结果以吹扫捕集-气质联用为平台检测生物样品中13种目标化合物时,在0.045 ng/mL-5.76 ng/mL浓度范围内,线性系数均大于0.995,血样进样量为5.0 mL时,方法检出限为0.03 ng/mL-0.58 ng/mL。加标回收率为81.4%-117.8%,RSD为2.5%-12.3%。尿液进样量为30.0mL时,方法检出限为0.006ng/mL-0.15 ng/mL,加标回收率为76.3%-105.1%,RSD为1.7%-11.2%。以固相微萃取-气质联用为平台,检测血样中13种目标化合物时,在0.045 ng/mL-5.76 ng/mL的浓度范围内,线性系数均大于0.995,血样进样量为5.0 mL时,方法检出限为0.03 ng/mL-0.58ng/mL,加标回收率为 84.4%-121.9%,RSD 为 1.7%-12.5%。使用吹扫捕集-气质联用检测31份血样中挥发性有机物,邻二甲苯浓度为0.091 ng/mL-0.194 ng/mL,乙苯浓度为 0.099 ng/mL-0.189 ng/mL,甲苯浓度为 0.492 ng/mL-1.512 ng/mL,苯浓度为 0.072 ng/mL-1.355 ng/mL,间对二甲苯浓度为 0.172 ng/mL-4.152 ng/mL。使用吹扫捕集-气质联用检测38份尿样中挥发性有机物,邻二甲苯浓度范围在0.023 ng/mL-0.214 ng/mL,乙苯浓度范围在0.101 ng/mL-0.218 ng/mL,甲苯浓度范围在0.034 ng/mL-0.124 ng/mL,间对二甲苯浓度范围在0.089 ng/mL-0.215 ng/mL。使用固相微萃取测定9份血液中挥发性有机物,邻二甲苯浓度范围在0.147 ng/mL-0.241 ng/mL,甲苯浓度范围在0.114 ng/mL-0.257 ng/mL,苯浓度为 0.306 ng/mL-0.324 ng/mL,间对二甲苯浓度范围在 0.145 ng/mL-0.147 ng/mL。结论该研究解决了血、尿在吹扫过程中产生泡沫堵塞仪器的问题、降低了检测空白、减小了基质效应;适用于大量血、尿样品中挥发性有机物的常规检测;以吹扫捕集-气质联用为平台建立的检测方法成本低、方法易推广;以固相微萃取-气质联用为平台建立的检测方法效率高、操作简便。
[Abstract]:In order to grasp the basic situation of the main environmental pollution on the human health in key areas of China, the health risk caused by the environmental pollution was evaluated. The Ministry of Environmental Protection and the State Health and Planning Commission jointly organized the "Special investigation on Environment and Health in key areas of the country" (hereinafter referred to as "the Special investigation") in 2015-2017. The present study is part of a special investigation. Mainly responsible for the establishment of blood volatile organic compounds detection methods and laboratory quality control related work. Methods 13 kinds of volatile organic compounds (VOCs) in urine were determined on the basis of blowing and trapping combined with GC / MS and solid phase microextraction (SPME) as the experimental platform with defoamer and isotopic internal standard. The calibration curve was established by double dilution method and the volatile organic compounds in whole blood / urine were determined by blowing and trapping gas chromatography / mass spectrometry isotope internal standard method. Solid-phase microextraction-gas chromatography-mass spectrometry isotope internal standard method was used to detect volatile organic compounds in whole blood. Results 13 target compounds in biological samples were detected on the platform of purge trapping and gas chromatography-mass spectrometry. In the range of 0.045 ng/mL-5.76 ng/mL, the linear coefficients were all greater than 0.995, and the blood sample volume was 5.0 mL. The detection limit was 0.03 ng/mL-0.58 / mL. The recoveries were 81.4% -117.8%. The detection limit of the method was 0.006 ng / mL-0.15 ng/mL when the volume of urine sample was 30.0 mL. The recovery rate was 76.3- 105.1% RSD was 1.7- 11.2.The solid phase microextraction-GC-MS was used as a platform for the determination of 13 target compounds in blood samples. In the concentration range of 0.045 ng/mL-5.76 ng/mL, the linear coefficients were all greater than 0.995, and the blood sample volume was 5.0 mL. The detection limit was 0.03 ng / mL -0.58 ng 路mL ~ (-1), and the recovery rate was 84.4% -121.9%. The RSD was 1.7- 12.5. the volatile organic compounds in 31 blood samples were detected by purging and trapping combined with gas chromatography-mass spectrometry. The concentration of o-xylene was 0.091 ng/mL-0.194 / mL and ethylbenzene was 0.099 ng/mL-0.189 ng/mL. Toluene concentration was 0.492 ng/mL-1.512 / mL, benzene concentration was 0.072 ng/mL-1.355 ng/mL. The concentration of m-p-xylene was 0.172 ng/mL-4.152 / mL. The volatile organic compounds in 38 urine samples were determined by purging and trapping combined with GC-MS. The concentration range of o-xylene is 0.023 ng/mL-0.214 / mL and ethylbenzene is 0.101 ng/mL-0.218 ng/mL. The concentration of toluene was in the range of 0.034 ng/mL-0.124 ng/mL. The concentration of m-p-xylene was in the range of 0.089 ng/mL-0.215 ng / mL. Solid phase microextraction (SPME) was used to determine the volatile organic compounds (VOCs) in blood of 9 samples. The concentration of o-xylene was in the range of 0.147 ng/mL-0.241 / mL, and the concentration of toluene was in the range of 0.114 ng/mL-0.257 ng/mL. Benzene concentration was 0.306 ng/mL-0.324 ng/mL. The concentration of m-p-xylene was in the range of 0.145 ng/mL-0.147 / mL. Conclusion this study solves the problem of foam clogging in blood and urine during purging. The detection blank is reduced and the matrix effect is reduced. It is suitable for routine detection of volatile organic compounds in blood and urine samples. The detection method established on the platform of purging and trapping combined with gas chromatography has low cost and is easy to be popularized. The method based on solid-phase microextraction-GC-MS platform has high efficiency and simple operation.
【学位授予单位】：中国疾病预防控制中心
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：R446.1;O657.63

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