果蔗中3-硝基丙酸分子印迹固相微萃取分离、纯化及高效液相色谱测定研究

发布时间：2018-03-17 12:28

本文选题：果蔗　切入点：3-硝基丙酸　出处：《华中农业大学》2017年硕士论文　论文类型：学位论文

【摘要】：(1)中国南方盛产甘蔗,并在冬季和夏季通过运输、贮藏并且销售国内外。但是果蔗在潮湿环境贮藏过程中容易感染真菌从而产生“霉变”,生成3-硝基丙酸(3-NPA),这是一种果蔗的最有名的毒素之一。而食用含有这种真菌毒素的果蔗会对消费者的身体健康造成持续性的威胁。本研究通过测定来自中国12个省的甘蔗样品表面3-NPA的浓度,并在此基础上建立了3-NPA的模型轮廓。通过液-液萃取(LLE)的方法提取了甘蔗中的3-NPA,之后用HPLC分离纯化3-NPA,并在210 nm波长处检测定量。随后用液质联用(LC-MS)手段和核磁共振(NMR)对分离纯化后的3-NPA进行绝对定性,确定其分子结构。标准曲线结果表明,该物质呈现很好的线性关系,和相关系数(r=0.9999),检测限和定量限分别达到了0.0023 mg/kg和0.0066 mg/kg。样品平均回收率分布于99.85%到101%之间,相对标准偏差为0.41%(n=12)。另外,来自中国更远省市如山东省、广东省、海南省和吉林省得甘蔗样品中3-NPA的浓度高达80 mg/kg,并显著高于其他省市。但是来自湖北武汉地区的新鲜甘蔗样品中3-NPA的浓度最低(45.5 mg/kg)。该结果表明除了温度这一因素以外,甘蔗的贮藏和运输过程也是造成3-NPA富集的主要决定因素。(2)如今农产品农产品加工和食品安全的控制越来越依赖先进的分析手段来用于农产品加工和食品安全的控制。本研究也制备了一种基于分子印记聚合物(MIPs)的新的选择性材料,它在本体聚合手段的基础上进一步利用固相萃取(SPE)方法来富集甘蔗表面的3-NPA,随后利用HPLC进一步纯化分离纯化。本研究的目的在于通过MIP和SPE手段,建立一种分离纯化、清除、预富集3-NPA的方法,并制备该材料。该制备后的材料通过场发射扫描电镜表征,并通过傅里叶红外光谱(FT-IR)进一步表征,最后测定SA-SMIP的吸附容量。本研究建立的MISPE方法在40~70 mg/L内表现出良好的线性,相关系数为(r2)0.9992,并且回收率高达99%,该方法LOD和LOG检测限分别达到了0.19 mg/L和0.58mg/L。该方法成功用于检测分析甘蔗样品中3-NPA含量。MIP-SPE不但可以用于目标3-NPA的预富集过程,也能够有效去除样品基质中其他物质的干扰。该MISPE技术成功用于毒性甘蔗中3-NPA的分离纯化、预富集及清除过程。
[Abstract]:Southern China is rich in sugar cane, which is transported through winter and summer. Stored and sold at home and abroad. But sugarcane is susceptible to fungal infection during storage in humid conditions, resulting in "mildew", which is one of the most famous toxins in fruit cane, which is produced by 3-nitropropionate, which is one of the most famous toxins in fruit cane. And eating contains this true. This study measured the concentration of 3-NPA on the surface of sugarcane samples from 12 provinces in China. On this basis, the model profile of 3-NPA was established. The 3-NPA was extracted from sugarcane by liquid-liquid extraction (LLEL) method, then purified by HPLC, and determined at 210nm wavelength. Then the method of liquid-mass spectrometry (LC-MS) and nuclear magnetic resonance (NMR) were used to detect the quantification of 3-NPA. The purified 3-NPA was determined by NMRs. The standard curve showed a good linear relationship with the correlation coefficient of 0.99999.The detection limit and the quantitative limit were 0. 0023 mg/kg and 0. 0066 mg / kg, respectively. The average recoveries of the samples ranged from 99.85% to 101%. The relative standard deviation is 0.41%. In addition, it comes from more distant provinces and cities in China, such as Shandong Province, Guangdong Province, The concentration of 3-NPA in sugarcane samples from Hainan Province and Jilin Province was as high as 80 mg / kg, which was significantly higher than that of other provinces and cities. However, the concentration of 3-NPA in fresh sugarcane samples from Wuhan area of Hubei Province was the lowest (45.5 mg / kg 路kg ~ (-1)). The results showed that besides temperature, the concentration of 3-NPA was 45.5 mg / kg 路kg ~ (-1). Storage and transportation of sugarcane is also the main determinant of 3-NPA enrichment.) nowadays, agricultural products processing and food safety control rely more and more on advanced analytical methods to control agricultural products processing and food safety. A new selective material based on molecular imprinted polymer (MIPs) was also prepared. The method of solid phase extraction (SPE) was used to enrich 3-NPAs on sugarcane surface and then purified by HPLC. The purpose of this study was to establish a method of separation and purification by means of MIP and SPE. The prepared material was characterized by field emission scanning electron microscopy (SEM) and further characterized by Fourier transform infrared spectroscopy (FTIR). Finally, the adsorption capacity of SA-SMIP was determined. The MISPE method developed in this study showed a good linearity in the range of 40 ~ 70 mg/L. The correlation coefficient was 0.9992 and the recovery rate was as high as 990.The detection limit of LOD and LOG reached 0.19 mg/L and 0.58 mg / L respectively. The method was successfully used to detect and analyze the content of 3-NPA in sugarcane samples. MIP-SPE could not only be used in the preconcentration process of target 3-NPA. The MISPE technique has been successfully used in the separation, purification, preconcentration and clearance of 3-NPA from toxic sugarcane.
【学位授予单位】：华中农业大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.72;TS255.7

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