發(fā)布時(shí)間：2018-01-08 20:17

  本文關(guān)鍵詞：人體血尿中揮發(fā)性有機(jī)物檢測(cè)方法建立及應(yīng)用　出處：《中國(guó)疾病預(yù)防控制中心》2017年碩士論文　論文類(lèi)型：學(xué)位論文

  更多相關(guān)文章： 生物樣品 揮發(fā)性有機(jī)物 吹掃捕集 固相微萃取 GC/MS同位素內(nèi)標(biāo)

【摘要】：為掌握我國(guó)重點(diǎn)地區(qū)主要環(huán)境污染對(duì)人群健康影響的基本狀況,評(píng)估環(huán)境污染帶來(lái)的健康風(fēng)險(xiǎn),環(huán)保部會(huì)同國(guó)家衛(wèi)計(jì)委于2015-2017年聯(lián)合組織開(kāi)展“全國(guó)重點(diǎn)地區(qū)環(huán)境與健康專(zhuān)項(xiàng)調(diào)查”(以下簡(jiǎn)稱(chēng)“專(zhuān)項(xiàng)調(diào)查”)。本研究作為專(zhuān)項(xiàng)調(diào)查的一部分,主要負(fù)責(zé)建立血中揮發(fā)性有機(jī)物檢測(cè)方法和實(shí)驗(yàn)室質(zhì)量控制相關(guān)工作。目的建立血、尿中13種揮發(fā)性有機(jī)物(VOCs)的檢測(cè)方法。方法以吹掃捕集-氣質(zhì)聯(lián)用和固相微萃取-氣質(zhì)聯(lián)用為實(shí)驗(yàn)平臺(tái),使用消泡劑和同位素內(nèi)標(biāo),在高純氮?dú)猸h(huán)境下處理樣品,采用“倍比稀釋法”建立校準(zhǔn)曲線(xiàn),建立了吹掃捕集-氣相色譜/質(zhì)譜-同位素內(nèi)標(biāo)法檢測(cè)全血/尿中揮發(fā)性有機(jī)物、固相微萃取-氣相色譜/質(zhì)譜-同位素內(nèi)標(biāo)法檢測(cè)全血中揮發(fā)性有機(jī)物三種檢測(cè)方法。結(jié)果以吹掃捕集-氣質(zhì)聯(lián)用為平臺(tái)檢測(cè)生物樣品中13種目標(biāo)化合物時(shí),在0.045 ng/mL-5.76 ng/mL濃度范圍內(nèi),線(xiàn)性系數(shù)均大于0.995,血樣進(jìn)樣量為5.0 mL時(shí),方法檢出限為0.03 ng/mL-0.58 ng/mL。加標(biāo)回收率為81.4%-117.8%,RSD為2.5%-12.3%。尿液進(jìn)樣量為30.0mL時(shí),方法檢出限為0.006ng/mL-0.15 ng/mL,加標(biāo)回收率為76.3%-105.1%,RSD為1.7%-11.2%。以固相微萃取-氣質(zhì)聯(lián)用為平臺(tái),檢測(cè)血樣中13種目標(biāo)化合物時(shí),在0.045 ng/mL-5.76 ng/mL的濃度范圍內(nèi),線(xiàn)性系數(shù)均大于0.995,血樣進(jìn)樣量為5.0 mL時(shí),方法檢出限為0.03 ng/mL-0.58ng/mL,加標(biāo)回收率為 84.4%-121.9%,RSD 為 1.7%-12.5%。使用吹掃捕集-氣質(zhì)聯(lián)用檢測(cè)31份血樣中揮發(fā)性有機(jī)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(duì)二甲苯濃度為 0.172 ng/mL-4.152 ng/mL。使用吹掃捕集-氣質(zhì)聯(lián)用檢測(cè)38份尿樣中揮發(fā)性有機(jī)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(duì)二甲苯濃度范圍在0.089 ng/mL-0.215 ng/mL。使用固相微萃取測(cè)定9份血液中揮發(fā)性有機(jī)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(duì)二甲苯濃度范圍在 0.145 ng/mL-0.147 ng/mL。結(jié)論該研究解決了血、尿在吹掃過(guò)程中產(chǎn)生泡沫堵塞儀器的問(wèn)題、降低了檢測(cè)空白、減小了基質(zhì)效應(yīng);適用于大量血、尿樣品中揮發(fā)性有機(jī)物的常規(guī)檢測(cè);以吹掃捕集-氣質(zhì)聯(lián)用為平臺(tái)建立的檢測(cè)方法成本低、方法易推廣;以固相微萃取-氣質(zhì)聯(lián)用為平臺(tái)建立的檢測(cè)方法效率高、操作簡(jiǎn)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(xué)位授予單位】：中國(guó)疾病預(yù)防控制中心
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類(lèi)號(hào)】：R446.1;O657.63

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