本文選題：石斑魚 + 阿維菌素類藥物殘留　； 參考：《食品科學(xué)》2017年22期

【摘要】：建立高效液相色譜-串聯(lián)質(zhì)譜同時(shí)定量檢測(cè)石斑魚血漿、肌肉組織、肝臟組織中阿維菌素、伊維菌素、甲氨基阿維菌素苯甲酸鹽方法。樣品經(jīng)乙腈提取,堿性氧化鋁固相萃取柱和LC-C18固相萃取柱串聯(lián)凈化,Thermo Hypersil Gold C18色譜柱分離,10 mmol/L乙酸銨-0.1%甲酸溶液和乙腈梯度洗脫,電噴霧正離子模式下以多反應(yīng)監(jiān)測(cè)方式檢測(cè),基質(zhì)匹配法外標(biāo)定量。分別以環(huán)境水體中阿維菌素上下限質(zhì)量濃度(4、8 ng/mL)、伊維菌素上下限質(zhì)量濃度(6、12 ng/mL)作為受試質(zhì)量濃度開展生物富集、消除實(shí)驗(yàn),并對(duì)石斑魚的食用安全進(jìn)行了風(fēng)險(xiǎn)評(píng)估。結(jié)果表明,阿維菌素和伊維菌素在2.5~200 ng/mL范圍內(nèi),甲氨基阿維菌素苯甲酸鹽在0.25~20 ng/mL范圍內(nèi),線性回歸系數(shù)均大于0.99。方法檢出限分別為2.5、2.5、0.25 ng/mL(血漿),1、1、0.1μg/kg(肌肉組織),2.5、2.5、0.25μg/kg(肝臟組織),方法定量限分別為5、5、0.5 ng/mL(血漿),2、2、0.2μg/kg(肌肉組織),5、5、0.5μg/kg(肝臟組織)。3個(gè)添加量的平均回收率為74.6%~93.6%,日內(nèi)相對(duì)標(biāo)準(zhǔn)偏差為2.3%~10.9%,日間相對(duì)標(biāo)準(zhǔn)偏差為9.2%~12.6%。阿維菌素、伊維菌素均屬于非生物累積性物質(zhì),在石斑魚體內(nèi)代謝規(guī)律相同,均按一級(jí)動(dòng)力學(xué)過(guò)程從體內(nèi)消除。本研究條件下,環(huán)境水體中藥物質(zhì)量濃度是石斑魚肌肉組織中藥物殘留質(zhì)量濃度及消除時(shí)間的重要因素。為保證食用安全,環(huán)境水體中阿維菌素質(zhì)量濃度達(dá)到4~8 ng/mL時(shí),石斑魚浸浴72 h后安全食用時(shí)間為22 d;環(huán)境水體中伊維菌素質(zhì)量濃度達(dá)到6~12 ng/mL時(shí),石斑魚浸浴72 h后安全食用時(shí)間為39 d。
[Abstract]:A high performance liquid chromatography-tandem mass spectrometry (HPLC / MS) method was developed for the simultaneous determination of abamectin, ivermectin and aminoabamectin benzoate in plasma, muscle and liver of grouper. The samples were extracted by acetonitrile, then purified by LC-C18 column and alkaline alumina solid-phase extraction column. Ten mmol/L ammonium acetate -0.1% formic acid solution and acetonitrile gradient elution were separated on Thermo Hypersil Gold C18 column. The results were detected by multi-reaction monitoring under electrospray positive ion mode. External standard quantification by matrix matching method. The concentration of abamectin at the upper and lower limits of abamectin and the concentration of ivermectin at the upper and lower limits of abamectin and ivermectin were used as bioconcentration and elimination experiments, respectively. The food safety of grouper was evaluated. The results showed that the linear regression coefficients of avermectin and ivermectin in the range of 2.5 ~ 200 ng/mL and methylamino abamectin benzoate in the range of 0.25 ~ 20 ng/mL were all greater than 0.99. Methods the detection limit was 2. 5 / 2. 5 ~ 2. 5ng / mL (plasma) = 0.1 渭 g / kg (muscle tissue = 2. 5 / 2. 5g / kg). (liver tissue). The quantitative limit of the method was 5 ~ 5ng / mL (plasma) = 22. 0. 2 渭 g / mL (muscle tissue = 55 / g / mL). The average recovery of the added dose was 93. 6% in liver tissue, 93. 6% in liver tissue, 2. 310.9% in intraday standard deviation, and 2. 310.9% in intraday time, respectively, and the average recovery was 93. 6 渭 g / kg in liver tissue (liver tissue), and the relative standard deviation was 2. 310.9% in intraday time (RSDs = 2 310.9%). The relative standard deviation was 9. 2% and 12. 6%. Avermectin and ivermectin are non-bioaccumulative substances, which have the same metabolic law in grouper and are eliminated from the body according to the first-order kinetic process. In this study, the mass concentration of drugs in environmental water was an important factor of drug residue concentration and elimination time in muscle tissue of grouper. In order to ensure food safety, when the mass concentration of abamectin in environmental water reaches 4 ~ 8 ng/mL, the safe eating time of grouper is 22 days after 72 h immersion, and the concentration of Ivermectin in environmental water reaches 6 ~ 12 ng/mL. The safe eating time of grouper was 39 days after 72 h immersion.
【作者單位】： 廈門大學(xué)材料學(xué)院;福建省水產(chǎn)研究所福建省海洋生物增養(yǎng)殖與高值化利用重點(diǎn)實(shí)驗(yàn)室;
【基金】：福建省海洋經(jīng)濟(jì)創(chuàng)新發(fā)展區(qū)域示范項(xiàng)目(閩臺(tái)重要海洋生物資源高值化開發(fā)技術(shù)公共服務(wù)平臺(tái),2014FJPT01) 廈門南方海洋研究中心項(xiàng)目(福建重要海洋經(jīng)濟(jì)生物種質(zhì)庫(kù)與資源高效開發(fā)技術(shù)公共服務(wù)平臺(tái),14PZY017NF17) 福建省海洋與漁業(yè)科技項(xiàng)目(KJXH-2010-007) 福建省海洋高新產(chǎn)業(yè)發(fā)展專項(xiàng)(閩海洋高新[2014]18號(hào)) 國(guó)家海洋局海洋公益性行業(yè)科研專項(xiàng)(201505034-4)
【分類號(hào)】：R155.5

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