本文選題：異菌脲 + 農(nóng)藥殘留��； 參考：《昆明醫(yī)科大學(xué)》2017年碩士論文

【摘要】：[目的]通過采用超高效液相色譜串聯(lián)質(zhì)譜法(UHPLC-MS/MS)測定云南省某縣農(nóng)村居民尿液及其居住環(huán)境的土壤、水體中的農(nóng)藥殘留情況,探討居民尿液中農(nóng)藥殘留量與農(nóng)藥使用情況、使用時(shí)采取防護(hù)措施的情況、自我報(bào)告與使用農(nóng)藥有關(guān)的癥狀及環(huán)境中農(nóng)藥殘留之間的關(guān)系,為農(nóng)藥殘留的體內(nèi)暴露提供直接證據(jù),為評估農(nóng)藥暴露健康風(fēng)險(xiǎn)提供依據(jù)。[方法]采用問卷調(diào)查和實(shí)驗(yàn)室檢測兩種研究方法,現(xiàn)場圍繞居民農(nóng)藥使用情況、使用時(shí)采取防護(hù)措施以及不適癥狀的出現(xiàn)等情況對230名居民開展問卷調(diào)查并采集其尿樣;同時(shí)采集29份土樣、28份水樣,采用UHPLC-MS/MS測定其中的17種農(nóng)藥。尿樣經(jīng)SPE(Waters Oasis MCX,3cc)柱固相提取,用甲醇和5%的氨水甲醇溶液洗脫后離心濃縮;水樣經(jīng)冷凍干燥;土樣經(jīng)甲醇提取,過濾后濃縮。所有樣品經(jīng)乙腈定容后,經(jīng)0.22 μm過濾器過濾,以0.01%的甲酸乙腈溶液和0.01%的甲酸水溶液為流動(dòng)相梯度洗脫,經(jīng)Cosmosil packed column(4.6 mm × 150 mm)色譜柱分離,采用電噴霧離子源正離子模式進(jìn)行質(zhì)譜檢測;用Analyst 1.6.2軟件分析離子流圖和質(zhì)譜圖,EpiData 3.1錄入問卷,SPSS 17.0進(jìn)行一般性描述分析和檢驗(yàn)。[結(jié)果]UHPLC-MS/MS方法的線性范圍為0.01-1.00 μg/mL,相關(guān)系數(shù)(r)均大于0.990;230份尿樣中檢測出多菌靈、異菌脲、百菌清、福美雙、甲氰菊酯、高效氯氟氰菊酯、毒死蜱7種農(nóng)藥殘留,本次共檢出150人尿液中有農(nóng)藥殘留,檢出陽性率為65.22%,其中異菌脲的檢出率最高,共檢出102份,檢出陽性率為44.35%。尚未發(fā)現(xiàn)居民尿液中農(nóng)藥殘陽性率及殘留濃度在性別、年齡等不同分組間有差別;兩個(gè)鄉(xiāng)鎮(zhèn)的居民尿液中農(nóng)藥殘留檢出陽性率有差別(χ2=7.29,P0.05);五個(gè)村莊間居民尿液中農(nóng)藥殘留及異菌脲殘留檢出陽性率均有差別(χ2=10.91,χ2=11.49,P0.05),陽性人群尿液中異菌脲殘留濃度有差別(F =3.60,P0.01)。居民中最近一個(gè)月未使用農(nóng)藥的人群尿液中農(nóng)藥殘留陽性率低于使用人群(χ2=10.59,P0.05);尿液中異菌脲殘留陽性人群中,未使用農(nóng)藥人群尿液中異菌脲殘留農(nóng)藥濃度低于使用人群(t=5.78,P0.05)。尿液中未檢出農(nóng)藥殘留人群在使用農(nóng)藥時(shí)佩戴口罩、橡膠手套、防護(hù)服、穿高筒雨鞋的頻率高于檢出人群(Z =-4.969,Z =-5.359,Z =-5.180,Z=-2.783,P0.01),防護(hù)頻率高的人群尿液中異菌脲殘留檢出率(χ2=24.74,P0.001)、殘留濃度(F=3.35,P0.05)均較低。沒有出現(xiàn)農(nóng)藥意外皮膚接觸的人群尿液中農(nóng)藥殘留檢出率低于有過農(nóng)藥意外皮膚接觸的人群(χ2 =6.11,P0.05),農(nóng)藥皮膚意外接觸后及時(shí)清洗的人群尿中農(nóng)藥殘留檢出率低于未處理者(χ2=10.45,P0.05)。農(nóng)藥殘留檢出陽性人群出現(xiàn)頭暈/頭昏、頭疼、惡心、皮膚發(fā)癢的頻率多于檢出陰性人群(χ2=4.41,χ2=3.86,χ2=7.10,χ2 =6.25,P0.05)。土樣中檢出多菌靈、異菌脲、毒死蜱這3種農(nóng)藥殘留,殘留濃度范圍為0.05-0.76 μg/mL,共檢出12份土樣中有農(nóng)藥殘留,檢出陽性率為41.38%,其中大田土檢出陽性率為53.33%,自留地土樣檢出陽性率為28.57%。三種農(nóng)藥中檢出例數(shù)最多的是異菌脲,檢出8份,檢出陽性率為27.58%。水樣中檢出多菌靈和甲氰菊酯2種農(nóng)藥殘留,殘留濃度范圍為0.04-0.89μg/mL,共檢出7份水樣中有農(nóng)藥殘留,檢出陽性率為25.00%,其中灌溉水檢出陽性率為35.71%,飲用水水樣檢出陽性率為14.29%。兩種農(nóng)藥中檢出例數(shù)最多的是異菌脲,檢出5份,檢出陽性率為17.85%。[結(jié)論]該地居民尿液及其居住環(huán)境的水體與土壤樣本中均有農(nóng)藥殘留檢出,且都檢出有異菌脲殘留,殘留例數(shù)均最多。居民尿液中農(nóng)藥殘留檢出率較高,找出了農(nóng)藥殘留在體內(nèi)暴露的直接證據(jù),為評估農(nóng)藥暴露風(fēng)險(xiǎn)和環(huán)境影響提供了依據(jù)。使用農(nóng)藥時(shí)采取防護(hù)措施能有效的減少農(nóng)藥與人體的接觸,減少農(nóng)藥進(jìn)入人體,應(yīng)促使居民合理使用農(nóng)藥,加強(qiáng)使用農(nóng)藥時(shí)的自身防護(hù)措施,從而減少農(nóng)藥進(jìn)入人體,減少農(nóng)藥對健康的危害。
[Abstract]:[Objective] to determine the pesticide residues in the urine of the rural residents and their living environment in a county of Yunnan province by using the ultra high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS), to discuss the situation of pesticide residues in the urine and the use of pesticides in the urine of the residents, and to take protective measures when used. Self reports are related to the use of pesticides. The relationship between the symptoms and the pesticide residues in the environment provides direct evidence for the exposure of pesticide residues in the body and provides the basis for assessing the health risk of pesticide exposure. [Methods] two research methods are adopted by questionnaire survey and laboratory testing. A questionnaire survey was conducted for 230 residents and their urine samples were collected; 29 samples and 28 samples were collected and 17 kinds of pesticides were measured by UHPLC-MS/MS. The urine samples were extracted by solid phase of SPE (Waters Oasis MCX, 3cc) column, and after elution of methanol and 5% ammonia methanol solution; water samples were frozen and dried; soil samples were extracted by methanol and filtered. After acetonitrile constant volume, all samples were filtered by 0.22 micron M filter, 0.01% formic acid acetonitrile solution and 0.01% formic acid solution were eluted as mobile phase, and separated by Cosmosil packed column (4.6 mm x 150 mm) column, the electrospray ion source positive ion mode was used for mass spectrometry detection, and the ion flow was analyzed with Analyst 1.6.2 software. Map and mass spectrogram, EpiData 3.1 entered the questionnaire, SPSS 17 carried out general description analysis and test. [results]UHPLC-MS/MS method has a linear range of 0.01-1.00 mu g/mL, correlation coefficient (R) is greater than 0.990; 230 samples of urine samples were detected by carbendazim, carbendazide, chlorothalonil, methylene thruthrin, cyhalothrin, chlorpyrifos, 7 pesticide residues. The positive rate of the urine in 150 people was 65.22%, and the positive rate of isocarbamide was the highest, and the positive rate was 102. The positive rate of 44.35%. was not found in the urine of the residents in the urine and the residual concentration in the sex, age and other groups, and the pesticide residues in the urine of the two townships were detected. The positive rates of the positive rates were different (x 2=7.29, P0.05). The positive rates of pesticide residues in urine and residual urea residues in the urine of the five villages were different (x 2=10.91, X 2=11.49, P0.05), and the residual concentration of urea in urine was different (F =3.60, P0.01). The positive rate of pesticide residues in urine of the population who had not been used in the last month of the population was found. In the urine, the concentration of urea residues in urine was lower than that of the use group (t=5.78, P0.05). The frequency of the pesticide residues in urine was higher than that of the detected population (t=5.78, P0.05). Z =-4.969, Z =-5.359, Z =-5.180, Z=-2.783, P0.01), the detection rate of isocarbamide residues in urine of high protective frequency population (x 2=24.74, P0.001), the residual concentration (F=3.35, P0.05) were lower. The rate of pesticide residue detection in urine of people who had no accidental skin contact was lower than that of the population with the accidental skin contact of pesticide (chi 2). The detection rate of pesticide residues in urine of people who were cleaned in time after accidental contact of drug skin was lower than that of untreated people (x 2=10.45, P0.05). The positive population of pesticide residues appeared dizziness / dizziness, headache, nausea, and skin itching more frequently than negative people (x 2=4.41, X 2=3.86, Chi 2=7.10, chi 2 =6.25, P0.05). The residual concentration of chlorpyrifos was 0.05-0.76 micron g/mL, and a total of 12 samples of soil samples were detected. The positive rate was 41.38%. The positive rate of field soil detection was 53.33%, and the positive rate of soil samples was 28.57%. and three kinds of pesticides, the most of them was carbamide urea, 8 samples were detected, positive rate was 27.58%. water. 2 pesticides residue of Carbendazim and fenprothrin were detected in the sample. The residual concentration range was 0.04-0.89 mu g/mL, and 7 samples were detected in the water samples. The positive rate was 25%. The positive rate of irrigation water was 35.71%, the positive rate of drinking water samples was 14.29%. and two kinds of pesticides were the most common bacteria urea, and 5 samples were detected. The positive rate is 17.85%.[Conclusion] there are pesticide residues in the water and soil samples of the residents' urine and their living environment, and all the residual urea residues are detected. The number of residual cases is the most. The detection rate of pesticide residues in the urine is high, and the direct evidence of pesticide residues in the body is found out to assess the risk and environment of pesticide exposure. The influence provides the basis. When using the pesticide, the protection measures can effectively reduce the contact between the pesticide and the human body and reduce the pesticide into the human body. It should encourage the residents to use the pesticide rationally and strengthen the self-protection measures when using the pesticide, thus reducing the pesticide entry to the human body and reducing the harm to the health of the pesticide.

【學(xué)位授予單位】：昆明醫(yī)科大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：R12

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