本文選題：液相色譜串聯(lián)三重四級桿(LC-MS/MS)　切入點：親水性貝類毒素　出處：《青島大學》2017年碩士論文　論文類型：學位論文

【摘要】：目的:1.本研究課題建立14種親水性貝類毒素和11種親脂性貝類毒素的測定方法。2.測定當前青島市市售牡蠣、扇貝等貝類海產(chǎn)品中親水性貝類毒素和親水性貝類毒素的種類和含量,分析其時間變化規(guī)律,并進行風險評估。方法:1.14種親水性貝類毒素和11種親脂性貝類毒素測定方法的建立1%乙酸加熱提取樣品,再由石墨化炭黑固相萃取柱凈化后,液相色譜-串聯(lián)質(zhì)譜測定麻痹性貝類毒素,外標法定量。樣品組織經(jīng)100%甲醇提取,C18固相萃取柱凈化后,直接進樣用于游離態(tài)的親脂性貝類毒素以及軟骨藻酸測定,基質(zhì)加標校正,外標法定量。2.貝類海產(chǎn)品中貝類毒素的測定采集貝類樣品包括牡蠣、雜色蛤、縊蟶、蝦夷扇貝、櫛孔扇貝、貽貝、毛蚶、海螺、鈍擬蟹守螺、香螺和香波螺等樣品,12批次共計400個,樣品分成兩部分,一部分利用1%乙酸加熱提取,石墨化炭黑固相萃取柱凈化;另一部分則利用甲醇提取,C18固相萃取柱凈化提取,3.膳食消費量調(diào)查按24小時膳食回顧法問卷調(diào)查進行膳食習慣調(diào)查,對青島市某區(qū)的1104名居民進行調(diào)查,連續(xù)三天調(diào)查居民貝類食品消費量,記賬法記錄消耗量數(shù)據(jù)。4.結(jié)果分析方法計算采集樣品中貝類毒素種類和含量,分析不同時間樣品中貝類毒素的含量分布情況。采用日暴露法,計算膳食攝入貝類毒素的日膳食暴露量并進行風險評估。結(jié)果:1所建立的方法25種貝類毒素檢出限為4ug/kg~711ug/kg,精密度為0.8%~7.6%,平均回收率為85.2%~105.5%。2檢測樣品中貝類毒素種類和含量,其時間變化規(guī)律以及風險評估2.1檢測樣品中貝類毒素種類和含量,其時間變化規(guī)律本研究檢測12批次共計400份樣品,其中有73份有檢出,以親脂性貝類毒素為主,其檢出率為18.50%。其中,主要檢出成分有軟海綿酸(okadaic acid,OA)、蛤毒素(pectenotoxin-2,PTX-2)和蝦夷扇貝毒素YTXs(Yesssotoxin),其他種類的貝類毒素尚未檢出。檢出樣品中以扇貝和貽貝為主,其余種類樣品未檢出。貝類樣品的陽性檢出率隨時間變化而呈現(xiàn)一定差異,5-8月份貝類樣品中腹瀉性貝類毒素檢出率最高。OA在8月份檢出率最高,達29.20%,YTX在8月份檢出率最高,達26.80%,PTX-2在7月份檢出率最高,達35.20%,其中PTX-2最高含量為7.189μg/kg,尚未檢測出其他貝類毒素。2.2風險評估食用貝類體中的親脂性貝類毒素OA、PTX-2、YTX日暴露(攝人)量分別為0.48、0.88、0.65,按照膳食調(diào)查食用量水平下,尤其是夏秋季有可能會出現(xiàn)OA急性中毒事件,長期大劑量暴露其中有可能會威脅健康。食用含有YTX的貝類暴露量均在安全范圍內(nèi),暫時沒有其他危險影響。結(jié)論:1.所建立方法穩(wěn)定,回收率符合實驗要求,操作較為簡單,靈敏度和精密度滿足檢測確證。2.不同種貝類中毒素種類和含量不同,不同季節(jié)中貝類毒素含量不同。3.大多數(shù)貝類中存在貝類毒素污染的問題,根據(jù)檢測的目前市面貝類樣品中毒素的含量小于歐盟限量值,對人們生活暫時不構(gòu)成危害風險,但后續(xù)長期受到污染對人類健康是否存在影響有待進一步研究。
[Abstract]:Objective: a.2. method for determination of 1. this paper establishes 14 kinds of hydrophilic and lipophilic shellfish toxins 11 kinds of shellfish toxin determination currently sold in Qingdao City oysters, species and content such as hydrophilic Scallop in Shell shellfish shellfish toxins and hydrophilic shellfish toxins, analyze the time variation and risk assessment. Methods: extraction sample build 1% acetic acid heating method for the determination of 1.14 kinds of hydrophilic and lipophilic shellfish toxins 11 kinds of shellfish toxins, then by graphite carbon black solid phase extraction column purification, determination of paralytic shellfish toxin liquid chromatography tandem mass spectrometry, and quantified by external standard method. The sample tissue was extracted with 100% methanol, purified by C18 solid phase extraction column, directly the sample for free and lipophilic shellfish toxin domoic acid determination, matrix calibration, external standard method for quantitative.2. of shellfish toxins in shellfish seafood were collected in shellfish samples including oyster, Clam, Sinonovacula constricta, Yesso Scallop in Shell Scallop in Shell, Chlamys, mussel, clam, conch, blunt quasi cerithium, conch and shampoo snail samples, a total of 12 batches of 400 samples, divided into two parts, one part with 1% acetic acid extraction, graphitized carbon black solid phase extraction column purification; the other part is using methanol extraction, C18 solid phase extraction column purification extraction, 3. dietary consumption survey in 24 hour dietary recall questionnaire for dietary habits survey, conducted a survey of 1104 residents in a district of Qingdao City, three consecutive days of investigation of resident shellfish consumption accounts record data analysis of the results of.4. method to calculate the sample in shellfish species and content consumption, content distribution analysis of shellfish toxin in different time samples. By day exposure, dietary intake calculation of shellfish toxin exposure and risk assessment. Results: 1 of 25 Kind of shellfish toxin detection limit was 4ug/kg~711ug/kg, the precision is 0.8%~7.6%, the average recovery rate of 85.2%~105.5%.2 in the samples of shellfish toxin type and content, the time variation of risk assessment and 2.1 samples of shellfish toxin types and content of this study is to detect the time variation of the total of 12 batches of 400 samples, of which 73 samples are detected the lipophilic shellfish toxins, and the detection rate of 18.50%. among them, the main components of detection of okadaic acid (okadaic acid, OA), saxitoxin (pectenotoxin-2, PTX-2) and mizuhopecten Scallop in Shell toxin YTXs (Yesssotoxin), other types of shellfish toxins have not been detected. The detection of samples to Scallop in Shell and mussels, other species the samples were not detected in shellfish samples. The positive rate of change with time and showed some differences in the detection of diarrhetic shellfish poison in the highest rate of.OA in August was 5-8 in shellfish samples The highest rate reached 29.20%, the highest detection rate of YTX in August, PTX-2 in July reached 26.80%, the highest positive rate was 35.20%, the highest content of PTX-2 was 7.189 g/kg, has not yet been detected in other shellfish toxin.2.2 risk assessment of edible shellfish in lipophilic shellfish toxins OA, PTX-2, YTX (intake) amount of exposure are 0.48,0.88,0.65, the level of consumption in accordance with the dietary survey, especially there may be OA in acute poisoning in summer and autumn, the long-term high dose exposure which may be a threat to health. Food containing YTX shellfish exposure in the safe range, no effect. Other dangerous conclusion: 1. the method is stable, the recovery rate in line with the experimental requirements, the operation is simple, sensitivity and precision meet the test confirmed.2. of different types and different hormone content of shellfish poisoning, shellfish toxin content in different seasons have different.3. most in shellfish The pollution problem of shellfish poison is based on the detection of toxins in the market shellfish, which is less than the European limit. It does not pose a risk to people's lives. But whether the long-term pollution is affecting human health needs further study.

【學位授予單位】：青島大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：R155.5

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