發(fā)布時間：2018-01-08 20:17

  本文關鍵詞：人體血尿中揮發(fā)性有機物檢測方法建立及應用　出處：《中國疾病預防控制中心》2017年碩士論文　論文類型：學位論文

  更多相關文章： 生物樣品 揮發(fā)性有機物 吹掃捕集 固相微萃取 GC/MS同位素內標

【摘要】：為掌握我國重點地區(qū)主要環(huán)境污染對人群健康影響的基本狀況,評估環(huán)境污染帶來的健康風險,環(huán)保部會同國家衛(wèi)計委于2015-2017年聯合組織開展“全國重點地區(qū)環(huán)境與健康專項調查”(以下簡稱“專項調查”)。本研究作為專項調查的一部分,主要負責建立血中揮發(fā)性有機物檢測方法和實驗室質量控制相關工作。目的建立血、尿中13種揮發(fā)性有機物(VOCs)的檢測方法。方法以吹掃捕集-氣質聯用和固相微萃取-氣質聯用為實驗平臺,使用消泡劑和同位素內標,在高純氮氣環(huán)境下處理樣品,采用“倍比稀釋法”建立校準曲線,建立了吹掃捕集-氣相色譜/質譜-同位素內標法檢測全血/尿中揮發(fā)性有機物、固相微萃取-氣相色譜/質譜-同位素內標法檢測全血中揮發(fā)性有機物三種檢測方法。結果以吹掃捕集-氣質聯用為平臺檢測生物樣品中13種目標化合物時,在0.045 ng/mL-5.76 ng/mL濃度范圍內,線性系數均大于0.995,血樣進樣量為5.0 mL時,方法檢出限為0.03 ng/mL-0.58 ng/mL。加標回收率為81.4%-117.8%,RSD為2.5%-12.3%。尿液進樣量為30.0mL時,方法檢出限為0.006ng/mL-0.15 ng/mL,加標回收率為76.3%-105.1%,RSD為1.7%-11.2%。以固相微萃取-氣質聯用為平臺,檢測血樣中13種目標化合物時,在0.045 ng/mL-5.76 ng/mL的濃度范圍內,線性系數均大于0.995,血樣進樣量為5.0 mL時,方法檢出限為0.03 ng/mL-0.58ng/mL,加標回收率為 84.4%-121.9%,RSD 為 1.7%-12.5%。使用吹掃捕集-氣質聯用檢測31份血樣中揮發(fā)性有機物,鄰二甲苯濃度為0.091 ng/mL-0.194 ng/mL,乙苯濃度為 0.099 ng/mL-0.189 ng/mL,甲苯濃度為 0.492 ng/mL-1.512 ng/mL,苯濃度為 0.072 ng/mL-1.355 ng/mL,間對二甲苯濃度為 0.172 ng/mL-4.152 ng/mL。使用吹掃捕集-氣質聯用檢測38份尿樣中揮發(fā)性有機物,鄰二甲苯濃度范圍在0.023 ng/mL-0.214 ng/mL,乙苯濃度范圍在0.101 ng/mL-0.218 ng/mL,甲苯濃度范圍在0.034 ng/mL-0.124 ng/mL,間對二甲苯濃度范圍在0.089 ng/mL-0.215 ng/mL。使用固相微萃取測定9份血液中揮發(fā)性有機物,鄰二甲苯濃度范圍在0.147 ng/mL-0.241 ng/mL,甲苯濃度范圍在0.114 ng/mL-0.257 ng/mL,苯濃度為 0.306 ng/mL-0.324 ng/mL,間對二甲苯濃度范圍在 0.145 ng/mL-0.147 ng/mL。結論該研究解決了血、尿在吹掃過程中產生泡沫堵塞儀器的問題、降低了檢測空白、減小了基質效應;適用于大量血、尿樣品中揮發(fā)性有機物的常規(guī)檢測;以吹掃捕集-氣質聯用為平臺建立的檢測方法成本低、方法易推廣;以固相微萃取-氣質聯用為平臺建立的檢測方法效率高、操作簡便。
[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.
【學位授予單位】：中國疾病預防控制中心
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：R446.1;O657.63

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