【摘要】：果蔬在生長(zhǎng)和貯存過程中為了防止病蟲害及自身疾病,多被噴灑上一定量的農(nóng)藥,雖絕大部分會(huì)由于日曬、雨淋而流失,但在產(chǎn)品中仍殘留微量農(nóng)藥。農(nóng)藥殘留問題使我國果蔬在進(jìn)出口貿(mào)易中頻頻遭受技術(shù)壁壘的限制。因此,建立一種快速篩查果蔬農(nóng)藥殘留的檢測(cè)方法具有重要的現(xiàn)實(shí)意義。本研究依據(jù)121種農(nóng)藥在氣相色譜-質(zhì)譜中不同的保留時(shí)間,分為四組,根據(jù)每種農(nóng)藥不同的響應(yīng)值配制四組混合標(biāo)準(zhǔn)溶液,并為各組農(nóng)藥建立選擇離子監(jiān)測(cè)方法,依據(jù)保留時(shí)間和特征離子豐度比,對(duì)農(nóng)藥進(jìn)行確證,外標(biāo)法定量。樣品前處理采用乙腈提取,使用SPE固相萃取(Sep-Pak Carbon NH2固相萃取柱)凈化技術(shù)。實(shí)驗(yàn)用樣品空白基質(zhì)提取液配制基質(zhì)混合標(biāo)準(zhǔn)工作溶液,標(biāo)準(zhǔn)曲線的相關(guān)系數(shù)均高于0.996。農(nóng)藥的添加回收率在60.57%～117.64%之間,其中咪酰胺、吡氟草胺、甲苯氟磺胺、庚烯磷、敵敵畏的添加回收率在60%-70%之間,其他農(nóng)藥的添加回收率均在70%-120%之間,相對(duì)標(biāo)準(zhǔn)偏差均小于15%。方法檢出限的范圍為0.003～0.375mg/kg,有42種農(nóng)藥的檢出限低于國標(biāo)方法GB/T19648-2006。在38mmin完成一組農(nóng)藥的檢測(cè),即使用同一升溫程序,總共進(jìn)樣4次,就可以完成121種農(nóng)殘的檢測(cè),可滿足國內(nèi)及對(duì)外出口蔬菜等農(nóng)產(chǎn)品的農(nóng)殘檢測(cè)分析。本實(shí)驗(yàn)以黃瓜作為實(shí)驗(yàn)基質(zhì),對(duì)比選擇離子掃描總離子譜圖發(fā)現(xiàn),黃瓜提取液作為基質(zhì)配制標(biāo)準(zhǔn)物質(zhì)響應(yīng)值均高于或等于空白溶劑所配制的標(biāo)準(zhǔn)物質(zhì)響應(yīng)值。農(nóng)藥五氟苯、地茂散、六氯苯、α-BHC、五氯硝基苯、γ-BHC、異稻瘟凈、樂果、皮蠅磷、乙烯菌核利、毒死蜱、δ-BHC、環(huán)氧七氯、α-硫丹、p,p'-DDE、五氯苯受到基質(zhì)影響較小,基本可以忽略。其他標(biāo)準(zhǔn)物質(zhì)有明顯的基質(zhì)增強(qiáng)效應(yīng)。實(shí)驗(yàn)提取了黃瓜、白菜、蘋果3種基質(zhì)的基質(zhì)液,對(duì)比3種基質(zhì)對(duì)C組標(biāo)準(zhǔn)物質(zhì)的基質(zhì)效應(yīng)。基質(zhì)效應(yīng)的對(duì)比顯示不同的基質(zhì)對(duì)農(nóng)藥的基質(zhì)效應(yīng)是不同的。有些農(nóng)藥在3種基質(zhì)中的基質(zhì)效應(yīng)變化較大。所以,在實(shí)驗(yàn)中基質(zhì)效應(yīng)不可忽略,實(shí)驗(yàn)認(rèn)為用空白基質(zhì)溶液配制標(biāo)準(zhǔn)曲線是補(bǔ)償基質(zhì)效應(yīng)的比較好的辦法。
[Abstract]:In order to prevent diseases and insect pests and their own diseases, fruits and vegetables are mostly sprayed with certain amount of pesticides during growth and storage. Although most of them will be lost due to sun and rain, there are still traces of pesticides remaining in the products. The problem of pesticide residues frequently restricts the import and export of fruits and vegetables in China. Therefore, it is of great practical significance to establish a rapid screening method for pesticide residues in fruits and vegetables. According to the retention time of 121 pesticides in gas chromatography-mass spectrometry, this study was divided into four groups. According to the different response values of each pesticide, four groups of mixed standard solutions were prepared, and a selective ion monitoring method was established for each group of pesticides. According to retention time and characteristic ion abundance ratio, pesticide was confirmed and quantified by external standard method. The sample was extracted by acetonitrile and purified by SPE solid phase extraction (Sep-Pak Carbon NH2 solid phase extraction column). The correlation coefficient of the standard working solution was higher than 0.996 when the blank matrix extract of the sample was used to prepare the mixed standard working solution. The recoveries of pesticides were between 60.57% and 117.64%, and the recoveries of midamide, Piraclor, toluenesulfonamide, heptene and dichlorvos were between 60% and 70%, the recoveries of other pesticides were between 70% and 120%, and the relative standard deviations were all less than 15%. The detection limit of the method was 0.003 ~ 0.375 mg / kg, and the detection limit of 42 pesticides was lower than that of the national standard method GB/T19648-2006.. When a group of pesticides were tested by 38mmin, even with the same temperature program, a total of 4 samples were injected, which could be used to detect and analyze the agricultural residues of agricultural products such as vegetables and other agricultural products exported at home and abroad. In this experiment, cucumber was used as experimental substrate, and the response values of Cucumber extract as substrate were higher than or equal to those prepared by blank solvent. Pesticides pentafluorobenzene, dimeo powder, hexachlorobenzene, 偽-BHC, pentachloronitrobenzene, 緯-BHC, isorice blast net, dimethoate, dermatophos, ethylenes ribonucleus, chlorpyrifos, 未-BHC, epoxide heptachloro, 偽-endosulfan, pnpn-DDE-, pentachlorobenzene were less affected by matrix and could be neglected. Other reference materials have obvious matrix enhancement effects. The substrates of cucumber, cabbage and apple were extracted and the effects of three substrates on group C reference materials were compared. The contrast of matrix effect shows that the matrix effect of different matrix on pesticide is different. The matrix effects of some pesticides in the three substrates vary greatly. Therefore, the matrix effect can not be ignored in the experiment. It is considered that the standard curve prepared by blank matrix solution is a better way to compensate the matrix effect.
【學(xué)位授予單位】：大連海事大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：X839.2

【參考文獻(xiàn)】

相關(guān)期刊論文 前10條

1 王慧文;;高效液相色譜技術(shù)在藥品檢驗(yàn)中的應(yīng)用及進(jìn)展[J];安徽醫(yī)藥;2008年11期

2 胡小鐘;徐盈;胡德聰;;六溴環(huán)十二烷異構(gòu)體在洶魚體內(nèi)的濃度分布與生物累積特征[J];分析科學(xué)學(xué)報(bào);2008年02期

3 劉長(zhǎng)武,劉鳳枝,翟廣書,劉瀟威,買光熙,陳勇,王一茹;蔬菜水果中25種有機(jī)氯農(nóng)藥殘留快速檢測(cè)方法[J];環(huán)境科學(xué)學(xué)報(bào);2003年04期

4 陳浩,柳訓(xùn)才,李勝清,陳智東;蔬菜中高毒有機(jī)磷農(nóng)藥多殘留的檢測(cè)方法研究[J];食品科學(xué);2005年03期

5 賀家亮;李開雄;劉海燕;;高效液相色譜法在食品分析中的應(yīng)用[J];食品研究與開發(fā);2008年11期

6 洪蔚萍,陳枝華,楊忠強(qiáng);氣相色譜法同時(shí)檢測(cè)蔬菜中多種有機(jī)磷、擬除蟲菊酯類農(nóng)藥殘留[J];色譜;2004年03期

7 隋凱;李軍;衛(wèi)鋒;儲(chǔ)小剛;趙守成;王玉萍;;固相萃取-高效液相色譜法同時(shí)檢測(cè)大米中12種磺酰脲類除草劑的殘留[J];色譜;2006年02期

8 薄濤;詹順安;胡培斌;王穎;張之旭;李平;;液相色譜-質(zhì)譜聯(lián)用對(duì)復(fù)雜食品基質(zhì)中407種多農(nóng)藥殘留量的測(cè)定[J];分析測(cè)試學(xué)報(bào);2008年S1期

9 雷軍;李曉華;王巍巍;王海敏;鄭毅男;;毛細(xì)管氣相色譜測(cè)定人參中有機(jī)氯與擬除蟲菊酯20種農(nóng)藥的殘留[J];藥物分析雜志;2008年04期

10 陳蘇芳;唐朗;張光濤;王寧;丁情;舒濤;陳國元;;2009—2011年武漢市某市場(chǎng)果蔬農(nóng)藥殘留狀況調(diào)查及預(yù)防對(duì)策[J];職業(yè)與健康;2012年10期

相關(guān)碩士學(xué)位論文 前1條

1 黃寶勇;果蔬中農(nóng)藥多殘留的氣相色譜—質(zhì)譜方法與基質(zhì)效應(yīng)的研究[D];中國農(nóng)業(yè)大學(xué);2005年

，

本文編號(hào)：2279836