基于新型基质的苯并（α）芘MALDI-TOF分析方法

发布时间：2018-04-20 12:07

本文选题：苯并(α)芘 + 金属有机骨架材料　；参考：《天津科技大学》2017年硕士论文

【摘要】：苯并(α)花(Benzoapyrene)是一种由苯环和芘分子稠合而成的五环类多环芳烃化合物,通常存在于植物油、乳制品、烤鱼肉等多种食品中,它是世界公认的三大致癌物质之一,由于苯并(α)芘是痕量存在于十分复杂的基质里,这对检测造成了一定的难度。基质辅助激光解析电离飞行时间质谱(MALDI-TOF/MS)属于软电离技术,具有高通量筛选、简便的样品前处理等特性,且灵敏度高(能达到pmol),因此在检测技术领域得到了极大的应用。基于MALDI-TOF/MS的传统基质在低分子量区(m/z600)会产生干扰峰,因此开发出一种新的材料来作为MALDI-TOF/MS的基质来检测小分子具有重要的意义。本文通过溶剂热法合成了金属有机骨架材料MIL-101 (Fe),将制备的材料通过紫外-可见光谱(UV-Vis)、傅里叶红外光谱(FT-IR)、扫描电镜(SEM)和X-射线衍射(XRD)进行了一系列的表征。结果表明,合成的金属有机骨架材料其表面均匀,吸收波长符合仪器激光能量的要求。将其与传统的基质做对比同时检测苯并(α)芘,结果表明,金属有机骨架材料MIL-101 (Fe)所得到的质谱图较为干净。使用所合成的材料作为基质,优化了质谱条件和上机条件,获得的最优条件为:靶板选用Polished Steel,激光能量为66%,基质的悬浮剂为乙醇/0.1%TFA,基质的浓度为6 mg mL-1。在此条件下建立了苯并(α)芘的MALDI-TOF/MS检测方法,方法的最低检出限可以达到0.1μg·L-1,苯并(α)芘的线性范围为0.25-50μg·L-1,决定系数R2为0.9986,相对标准偏差RSD (n=15)小于9.9%。将所建立的方法对日常生活中食用的植物油:芝麻油,胡麻油,茶油和橄榄油进行检测,并进行了添加回收实验,添加的高中低水平分别为10、1和0.5 μgkg-1,实验结果显示,4种实际样品的添加回收率介于80.0%-114.8%之间,相对标准偏差RSD(n= 5)均小于13.7%,说明本实验所建立的方法有较高的准确度和重现性,可满足实际样品分析的需求。
[Abstract]:Benzoapyrene (伪) is a kind of pentacyclic polycyclic aromatic hydrocarbons (PAHs), which is composed of benzene ring and pyrene molecules. It is commonly found in vegetable oils, dairy products, roasted fish and other foods. It is recognized as one of the three carcinogens in the world. Because benzo (伪) pyrene is a very complex matrix, it is difficult to detect. Matrix assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF / MS) is a soft ionization technology with high throughput screening, simple sample pretreatment and high sensitivity. Traditional matrix based on MALDI-TOF/MS can produce interference peak in low molecular weight region. Therefore, it is very important to develop a new material to detect small molecules in MALDI-TOF/MS. In this paper, the organometallic skeleton material, MIL-101 FERD, was synthesized by solvothermal method. The prepared materials were characterized by UV-Vis-Vis, FTIR, SEM and X- ray diffractometry. The results show that the synthesized metal-organic skeleton material has uniform surface and absorption wavelength which meets the requirement of laser energy. Benzo (伪) pyrene was detected simultaneously by comparing it with the traditional matrix. The results showed that the mass spectrogram obtained from the organometallic skeleton material MIL-101 was relatively clean. Using the synthesized material as the matrix, the mass spectrum conditions and the computer conditions were optimized. The optimum conditions were as follows: the target plate was selected as Polished step, the laser energy was 66, the suspension of the matrix was ethanol / 0.1 and the concentration of the substrate was 6 mg mL ~ (-1). Under these conditions, a MALDI-TOF/MS method for the detection of benzo (伪) pyrene was established. The minimum detection limit of the method was 0.1 渭 g / L ~ (-1), the linear range of benzo (伪) pyrene was 0.25-50 渭 g / L ~ (-1), the determination coefficient R ~ (2) was 0.9986, and the relative standard deviation (RSD) was less than 9.9B. The established method was used to detect vegetable oils used in daily life: sesame oil, sesame oil, tea oil and olive oil. The experimental results show that the recoveries of the four kinds of samples are between 80.0-114.8% and the relative standard deviation (RSDN = 5) are less than 13.70.The results show that the method established in this experiment has high accuracy and reproducibility, and the relative standard deviation (RSDN = 5) is less than 13.7g 路kg ~ (-1), indicating that the method established in this experiment has high accuracy and reproducibility. Can meet the actual sample analysis requirements.
【学位授予单位】：天津科技大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.63;TS207.5

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