【摘要】：農(nóng)產(chǎn)品食品安全問題已在全世界范圍內(nèi)備受關(guān)注,鴨肉作為飼養(yǎng)量最大的水禽并且具有極高的營養(yǎng)價(jià)值,因而其抗生素濫用導(dǎo)致的食用安全問題更是人們關(guān)注的一個(gè)焦點(diǎn),因此研究鴨肉中抗生素殘留的快速檢測方法具有十分重要的意義。表面增強(qiáng)拉曼光譜(SERS)法因其具有簡便、快捷、靈敏度高等特點(diǎn),已被廣泛地應(yīng)用在許多領(lǐng)域中。本文主要采用表面增強(qiáng)拉曼光譜法結(jié)合化學(xué)計(jì)量學(xué)法對鴨肉中的三種大環(huán)內(nèi)酯類抗生素進(jìn)行了快速檢測研究,其主要研究內(nèi)容及結(jié)果如下:(1)SERS定性定量快速檢測鴨肉中螺旋霉素的殘留。研究采用OTR202作為SERS活性基底,建立了螺旋霉素水溶液的快速檢測定量分析模型,并以乙酸乙酯作為提取溶劑,確定了螺旋霉素的1622cm-1峰可以作為其在鴨肉提取液中殘留檢測的拉曼特征峰。然后進(jìn)一步利用SERS結(jié)合自適應(yīng)迭代重加權(quán)懲罰最小二乘法(air-PLS)快速檢測鴨肉中的螺旋霉素殘留,實(shí)驗(yàn)通過單因素分析法確定了最佳條件,并在此條件下建立了螺旋霉素濃度范圍介于4.0~50.0mg/L之間的鴨肉提取液加標(biāo)樣本的標(biāo)準(zhǔn)曲線,并獲得了良好的線性關(guān)系且線性回歸方程為y=26.681x+1233.5,決定系數(shù)R2=0.9802,最低檢測限為4mg/L,預(yù)測樣本的平均回收率為73.38%~105.25%。(2)SERS定性定量快速檢測鴨肉中替米考星的殘留。研究采用OTR202作為SERS活性基底,建立了替米考星水溶液的快速檢測定量分析模型,并以乙酸乙酯作為提取溶劑,經(jīng)正己烷除脂、氮?dú)獯党蟮玫进喨馓崛∫?確定了替米考星的1584cm-1峰可以作為其在鴨肉中殘留檢測的拉曼特征峰。然后利用SERS結(jié)合air-PLS快速檢測鴨肉中的替米考星殘留,實(shí)驗(yàn)通過單因素分析法確定了最佳條件,并在此條件下建立了替米考星濃度范圍介于2.0~50.0mg/L之間的鴨肉提取液加標(biāo)樣本的標(biāo)準(zhǔn)曲線,并獲得了良好的線性關(guān)系且線性回歸方程為y=0.0419x+0.8252,決定系數(shù)R2=0.9839,最低檢測限為2mg/L,預(yù)測樣本的平均回收率74.76%~102.59%。(3)SERS定性定量快速檢測鴨肉中吉他霉素的殘留。研究采用OTR202作為SERS活性基底,建立了吉他霉素水溶液的快速檢測定量分析模型,并以乙酸乙酯作為提取溶劑,經(jīng)正己烷除脂、氮?dú)獯党蟮玫进喨馓崛∫?確定了吉他霉素的1228和1268cm-1峰可以作為其在鴨肉中殘留檢測的拉曼特征峰。然后利用SERS結(jié)合air-PLS快速檢測鴨肉中的吉他霉素殘留,實(shí)驗(yàn)通過單因素分析法確定了最佳條件,并在此條件下建立了吉他霉素濃度范圍介于4.0~40.0mg/L之間的鴨肉提取液加標(biāo)樣本的標(biāo)準(zhǔn)曲線,并獲得了一定的線性關(guān)系且線性回歸方程為y=0.0119x+0.9409,決定系數(shù)R2=0.9232,最低檢測限為4mg/L,預(yù)測樣本的平均回收率104.44%~108.35%。研究表明,采用SERS結(jié)合air-PLS建立鴨肉中螺旋霉素、替米考星和吉他霉素殘留的快速檢測研究方法是可行的。
[Abstract]:The problem of food safety of agricultural products has been paid close attention to all over the world. As the largest amount of waterfowl and high nutritional value, duck meat is the focus of attention because of the food safety caused by the abuse of antibiotics. Therefore, it is of great significance to study the rapid detection of antibiotic residues in duck meat. Surface enhanced Raman spectroscopy (SERS) has been widely used in many fields because of its simplicity, rapidity and high sensitivity. In this paper, surface enhanced Raman spectroscopy and chemometrics were used to study the rapid detection of three macrolides in duck meat. The main contents and results were as follows: (1) SERS was used to determine the residue of spiramycin in duck meat. Using OTR202 as the active substrate of SERS, a rapid quantitative analysis model of spiramycin aqueous solution was established, and ethyl acetate was used as the extraction solvent. The 1622cm-1 peak of spiramycin can be used as the Raman characteristic peak for detection of spiramycin residues in duck meat extract. Then SERS combined with adaptive iterative heavy weight penalty least square (air-PLS) method was used to detect spiramycin residues in duck meat quickly. The best conditions were determined by single factor analysis. Under these conditions, the standard curve of the duck meat extract added with standard sample was established, in which the concentration of spiramycin ranged from 4.0 to 50 mg / L, and the concentration of spiramycin was in the range of 5.0 mg / L. A good linear relationship was obtained. The linear regression equation was YY 26.681x 1233.5, the determination coefficient R20.902, the lowest detection limit 4 mg / L, and the average recovery rate of predicted samples was 73.38 and 105.25.The (2) SERS was used to determine the residues of telmicosin in duck meat qualitatively and quantitatively. Using OTR202 as the active substrate of SERS, a rapid quantitative analysis model of temicoxin in aqueous solution was established, and ethyl acetate was used as the extraction solvent, and the duck meat extract was obtained after n-hexane degreasing and nitrogen blowing. The 1584cm-1 peak of telmicosin can be used as the Raman characteristic peak of its residual detection in duck meat. Then SERS and air-PLS were used to detect the tenmicosin residues in duck meat. The best conditions were determined by single factor analysis. Under these conditions, the standard curve of the duck meat extract added with standard samples with the concentration range of 2.0 ~ 50.0 mg / L of telmicoxacin was established. A good linear relationship was obtained, and the linear regression equation was: yttria 0.0419x 0.8252, the determination coefficient R2N 0.9839, the lowest detection limit being 2mg / L, the average recovery of predicted samples was 74.76102.59. (3) SERS was used to determine the residue of guitar mycin in duck meat. Using OTR202 as the active substrate of SERS, a rapid quantitative analysis model of guitar mycin aqueous solution was established. Ethyl acetate was used as the extraction solvent, and the duck meat extract was obtained after n-hexane degreasing and nitrogen blowing. The peaks of 1228 and 1268cm-1 of Guitamycin can be used as the Raman characteristic peaks of the residue detection in duck meat. Then SERS and air-PLS were used to detect the guitar mycin residues in duck meat. The best conditions were determined by single factor analysis. Under these conditions, the standard curve of the duck meat extract with standard sample was established, in which the concentration of guitar mycin ranged from 4.0 to 40.0 mg / L. A certain linear relationship was obtained, and the linear regression equation was Y = 0.0119x 0.9409, the determination coefficient was R220.9232, the lowest detection limit was 4 mg / L, and the average recovery rate of the predicted sample was 104.440.108.35. The results showed that it was feasible to establish a rapid method for the detection of spiramycin, telmicosin and guitar mycin residues in duck meat by SERS and air-PLS.
【學(xué)位授予單位】：江西農(nóng)業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：S859.84

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