基于納米材料的食品安全與品質(zhì)快速檢測方法的研究
發(fā)布時間：2018-08-11 20:40
【摘要】：由于食品安全事件的頻繁曝光,人們對于食品安全與品質(zhì)的關(guān)注程度與日俱增。傳統(tǒng)的實驗室檢測方法,雖然具有靈敏度高、檢測結(jié)果準(zhǔn)確可靠等優(yōu)點,但是同樣存在著檢測周期長,樣品前處理過程復(fù)雜繁瑣,檢測通量較低,儀器設(shè)備維護成本高,需要專業(yè)人員操作等不足,已無法滿足目前食品安全與品質(zhì)的檢測需求。電化學(xué)分析技術(shù)具有成本低廉、方便、易于操作、儀器易于自動化和小型化、靈敏度高、選擇性好等特點。酶聯(lián)免疫分析技術(shù)具有特異性好,簡單方便,易于實現(xiàn)自動化等優(yōu)勢。 本論文綜合使用了納米技術(shù)、電化學(xué)分析技術(shù)、酶聯(lián)免疫分析技術(shù)、磁分離技術(shù)等諸多領(lǐng)域的知識,開發(fā)了針對不同檢測對象的食品安全與品質(zhì)的快速檢測方法。使用功能性材料離子液體作為粘合劑替代傳統(tǒng)的石蠟油來構(gòu)建碳糊(carbon paste, CP)電極,并將其應(yīng)用于茶葉中抗氧化劑表沒食子兒茶素沒食子酸酯(epigallocatechin gallate, EGCG)的快速檢測；在碳糊離子液體(ionic liquid carbon paste, ILCP)電極的基礎(chǔ)之上,使用本體改性的方法在碳糊中摻雜金納米顆粒(Au nanoparticle, Au NP),制備出金納米顆粒修飾的碳糊離子液體(Au NP-ILCP)電極,該電極被用于快速檢測肉制品中的亞硝酸鹽殘留；成功使用絲網(wǎng)印刷技術(shù)制備了碳納米管與離子液體修飾的絲網(wǎng)印刷電極,并研究了該電極在重金屬離子快速檢測方面的性能；制備了磁珠微納顆粒,并通過化學(xué)修飾與生物結(jié)合的方式制備了免疫磁珠,引入了核酸純化系統(tǒng),并使用競爭免疫的原理,實現(xiàn)了對肉制品中瘦肉精克倫特羅(clenbuterol, CLB)的快速檢測。本文為電化學(xué)分析檢測技術(shù)中電極的制備和修飾方法提供了數(shù)據(jù)支持,為酶聯(lián)免疫分析技術(shù)的應(yīng)用提供了一種新的思路,對于研發(fā)具有自主知識產(chǎn)權(quán)的食品安全與品質(zhì)快速檢測儀器具有借鑒意義。 本文主要研究內(nèi)容、結(jié)果和結(jié)論如下： (1)使用本體改性的方法制備了以功能材料離子液體為原料的CP電極,并將該電極用于茶葉中主要抗氧化劑EGCG的快速檢測。ILCP電極在最優(yōu)條件下對于EGCG的檢測性能如下所示：1)對EGCG的檢測范圍為5×10-7～1.25×10-5mol/L,檢測下限為1.32×10-7mol/L;2) ILCP電極能連續(xù)檢測EGCG濃度的變化,具有顯著的抗鈍化效果；3)ILCP電極對于的常見EGCG類似物具有抗干擾特性；4)ILCP電極對EGCG的檢測具有一致性、重現(xiàn)性和穩(wěn)定性；5) ILCP電極能成功用于實際樣本茶湯中EGCG的檢測。 (2)使用本體改性的方法將納米材料Au NP引入到ILCP電極中,成功制備了AuNP-ILCP電極,并使用Au NP-ILCP電極對實際樣本中的亞硝酸鹽殘留實現(xiàn)了快速檢測。Au NP-ILCP電極在最優(yōu)的條件下對于亞硝酸鹽的檢測性能如下所示：1)檢測范圍分別為1.0×10-4～1.0×10-3mol/L(循環(huán)伏安法(cyclic voltommetry, CV))、1.0×10-6～2.0×10-4mol/L(差分脈沖伏安法(differential pulse voltommetry, DPV))以及7.6×10-6～1.4×10-4mol/L(電流時間曲線法(chronoamperometry, CA));2) Au-ILCP電極具備較強的抗干擾能力；3) Au NP-ILCP電極具備一致性、重現(xiàn)性和穩(wěn)定性以及抗鈍化能力。 (3)使用免疫磁珠結(jié)合核酸分離純化系統(tǒng)的磁珠自動運輸?shù)墓δ?實現(xiàn)了對肉類實際樣本(豬肉、豬肝)中瘦肉精CLB的快速檢測分析。實驗結(jié)果表明：1)磁珠形貌為球形,且粒徑均一、單分散性較好,平均粒徑為509nm；2)修飾后的磁珠仍然保持很強的磁性,在外界磁場的作用下,在1-2s內(nèi)迅速完成磁分離；3)整個檢測過程共耗時25min,線性檢測范圍為0.14～45.5ppb；4)將該檢測體系用于肉類實際樣品(豬肉、豬肝)的回收率測試,豬肉和豬肝中鹽酸克倫特羅的回收率分別為98.1%-106.1%,94.2%-109.0%。 (4)使用碳納米管以及離子液體作為功能材料制備了一種新型的絲網(wǎng)印刷(screen printed, SP)電極,并將其用于肉制品中的重金屬離子Pb2+和Cd2+殘留的快速檢測。SP電極對于重金屬離子Pb2+和Cd2+的檢測性能如下：1)Pb2+的線性響應(yīng)范圍為1.0～100.0ppb,Cd2+的線性響應(yīng)范圍為1.0～100.0ppb;2)干擾實驗的結(jié)果表明當(dāng)溶液中的常見離子濃度200倍于Pb2+和Cd2+時,Pb2+和Cd2+離子的電流響應(yīng)變化小于5%。同時新型的SP電極還具有較好的一致性和穩(wěn)定性。3)使用新型的SP電極對午餐肉以及火腿腸中的Pb2+和Cd2+成分進行回收率測試,午餐肉中Pb2+和Cd2+的回收率為97.1%-102.9%,98.8%-103.0%,火腿腸中Pb2+和Cd2+的回收率為98.5%～106.5%,96.0%-103.5%。
[Abstract]:Because of the frequent exposure of food safety incidents, people pay more and more attention to food safety and quality. Although traditional laboratory testing methods have the advantages of high sensitivity, accurate and reliable detection results, they also have the advantages of long detection cycle, complex sample pretreatment process, low detection flux, instrument and equipment maintenance. The electrochemical analysis technology has the characteristics of low cost, convenience, easy operation, easy automation and miniaturization of the instrument, high sensitivity and good selectivity. The enzyme-linked immunoassay technology has good specificity, simple and convenient, easy to realize. Automation and other advantages.
In this paper, nanotechnology, electrochemical analysis technology, enzyme-linked immunoassay technology, magnetic separation technology and many other fields of knowledge were used to develop a rapid detection method for food safety and quality of different detection objects. Ase (CP) electrode was applied to the rapid detection of epigallocatechin gallate (EGCG) in tea, and Au nanoparticles (Au N) were doped into the carbon paste by bulk modification on the basis of ionic liquid carbon paste (ILCP) electrode. Carbon paste ionic liquid (Au NP-ILCP) electrode modified with gold nanoparticles was prepared, which was used for rapid detection of nitrite residues in meat products. Silk screen printing electrode modified with carbon nanotubes and ionic liquids was successfully prepared by silk screen printing technology, and its performance in rapid detection of heavy metal ions was studied. In this paper, the preparation and modification of electrodes for electrochemical analysis of clenbuterol (CLB) in meat products were studied. The method provides data support and provides a new idea for the application of enzyme-linked immunoassay (ELISA), which can be used for reference in the research and development of food safety and quality rapid detection instrument with independent intellectual property rights.
The main contents, results and conclusions are as follows:
(1) The CP electrode based on ionic liquids was prepared by bulk modification and used for the rapid detection of EGCG in tea. Under the optimal conditions, the detection performance of ILCP electrode for EGCG was as follows: 1) The detection range of EGCG was 5 - 7 mol / L; 2) ILCP electrode can continuously detect the concentration of EGCG changes, has a significant anti-passivation effect; 3) ILCP electrode for common EGCG analogues has anti-interference characteristics; 4) ILCP electrode detection of EGCG has consistency, reproducibility and stability; 5) ILCP electrode can be successfully used in the actual sample of tea soup EGCG detection.
(2) AuNP-ILCP electrode was successfully prepared by introducing nano-AuNP into ILCP electrode by bulk modification method, and nitrite residue in real samples was rapidly detected by AuNP-ILCP electrode. The detection performance of AuNP-ILCP electrode for nitrite under the optimal conditions was as follows: 1) The detection range was 1. 0 6550 Very consistent, reproducible and stable, and anti passivation capability.
(3) Immunomagnetic beads combined with magnetic beads of nucleic acid separation and purification system were used to detect and analyze leptin CLB in meat samples (pork, pork liver). The results showed that: 1) the morphology of the magnetic beads was spherical, and the particle size was uniform, monodispersity was good, the average particle size was 509 nm; 2) the modified magnetic beads remained unchanged. Strong magnetism, under the action of external magnetic field, magnetic separation can be completed quickly within 1-2 seconds; 3) the whole detection process takes 25 minutes, the linear detection range is 0.14-45.5 ppb; 4) the detection system is applied to the actual meat samples (pork, pork liver) recovery test, the recovery of clenbuterol hydrochloride in pork and pork liver is 98.1% - 106.1%, respectively. 94.2%-109.0%.
(4) Using carbon nanotubes and ionic liquids as functional materials, a novel screen printed (SP) electrode was prepared and applied to the rapid detection of Pb2+ and Cd2+ residues in meat products. The linear response range of Cd2+ was 1.0-100.0 ppb at 0.0 ppb. 2) The results of interference experiments showed that the current response of Pb2+ and Cd2+ ions was less than 5% when the concentration of common ions in the solution was 200 times that of Pb2+ and Cd2 +. The new SP electrode also had good consistency and stability. 3) The new SP electrode was used for lunch meat and ham sausage. The recoveries of Pb2+ and Cd2+ in lunch meat were 97.1% - 102.9%, 98.8% - 103.0%, and those in ham sausage were 98.5% - 106.5%, 96.0% - 103.5%.
【學(xué)位授予單位】：浙江大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2014
【分類號】：TS207.3
本文編號：2178179
[Abstract]:Because of the frequent exposure of food safety incidents, people pay more and more attention to food safety and quality. Although traditional laboratory testing methods have the advantages of high sensitivity, accurate and reliable detection results, they also have the advantages of long detection cycle, complex sample pretreatment process, low detection flux, instrument and equipment maintenance. The electrochemical analysis technology has the characteristics of low cost, convenience, easy operation, easy automation and miniaturization of the instrument, high sensitivity and good selectivity. The enzyme-linked immunoassay technology has good specificity, simple and convenient, easy to realize. Automation and other advantages.
In this paper, nanotechnology, electrochemical analysis technology, enzyme-linked immunoassay technology, magnetic separation technology and many other fields of knowledge were used to develop a rapid detection method for food safety and quality of different detection objects. Ase (CP) electrode was applied to the rapid detection of epigallocatechin gallate (EGCG) in tea, and Au nanoparticles (Au N) were doped into the carbon paste by bulk modification on the basis of ionic liquid carbon paste (ILCP) electrode. Carbon paste ionic liquid (Au NP-ILCP) electrode modified with gold nanoparticles was prepared, which was used for rapid detection of nitrite residues in meat products. Silk screen printing electrode modified with carbon nanotubes and ionic liquids was successfully prepared by silk screen printing technology, and its performance in rapid detection of heavy metal ions was studied. In this paper, the preparation and modification of electrodes for electrochemical analysis of clenbuterol (CLB) in meat products were studied. The method provides data support and provides a new idea for the application of enzyme-linked immunoassay (ELISA), which can be used for reference in the research and development of food safety and quality rapid detection instrument with independent intellectual property rights.
The main contents, results and conclusions are as follows:
(1) The CP electrode based on ionic liquids was prepared by bulk modification and used for the rapid detection of EGCG in tea. Under the optimal conditions, the detection performance of ILCP electrode for EGCG was as follows: 1) The detection range of EGCG was 5 - 7 mol / L; 2) ILCP electrode can continuously detect the concentration of EGCG changes, has a significant anti-passivation effect; 3) ILCP electrode for common EGCG analogues has anti-interference characteristics; 4) ILCP electrode detection of EGCG has consistency, reproducibility and stability; 5) ILCP electrode can be successfully used in the actual sample of tea soup EGCG detection.
(2) AuNP-ILCP electrode was successfully prepared by introducing nano-AuNP into ILCP electrode by bulk modification method, and nitrite residue in real samples was rapidly detected by AuNP-ILCP electrode. The detection performance of AuNP-ILCP electrode for nitrite under the optimal conditions was as follows: 1) The detection range was 1. 0 6550 Very consistent, reproducible and stable, and anti passivation capability.
(3) Immunomagnetic beads combined with magnetic beads of nucleic acid separation and purification system were used to detect and analyze leptin CLB in meat samples (pork, pork liver). The results showed that: 1) the morphology of the magnetic beads was spherical, and the particle size was uniform, monodispersity was good, the average particle size was 509 nm; 2) the modified magnetic beads remained unchanged. Strong magnetism, under the action of external magnetic field, magnetic separation can be completed quickly within 1-2 seconds; 3) the whole detection process takes 25 minutes, the linear detection range is 0.14-45.5 ppb; 4) the detection system is applied to the actual meat samples (pork, pork liver) recovery test, the recovery of clenbuterol hydrochloride in pork and pork liver is 98.1% - 106.1%, respectively. 94.2%-109.0%.
(4) Using carbon nanotubes and ionic liquids as functional materials, a novel screen printed (SP) electrode was prepared and applied to the rapid detection of Pb2+ and Cd2+ residues in meat products. The linear response range of Cd2+ was 1.0-100.0 ppb at 0.0 ppb. 2) The results of interference experiments showed that the current response of Pb2+ and Cd2+ ions was less than 5% when the concentration of common ions in the solution was 200 times that of Pb2+ and Cd2 +. The new SP electrode also had good consistency and stability. 3) The new SP electrode was used for lunch meat and ham sausage. The recoveries of Pb2+ and Cd2+ in lunch meat were 97.1% - 102.9%, 98.8% - 103.0%, and those in ham sausage were 98.5% - 106.5%, 96.0% - 103.5%.
【學(xué)位授予單位】：浙江大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2014
【分類號】：TS207.3
【參考文獻】
相關(guān)期刊論文 前1條
1 程啟坤,阮宇成,王月根,劉維華,朱珩;綠茶滋味化學(xué)鑒定法[J];茶葉科學(xué);1985年01期
，本文編號：2178179
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