【摘要】：提出使用甲酸甲胺作為新型電離增強(qiáng)劑改善反相液相色譜-電噴霧質(zhì)譜(LC-ESI-MS)檢測(cè)甘油三酯靈敏度的方法。使用反相C_(18)色譜柱,以玉米油的異丙醇溶液為樣品,選擇文獻(xiàn)中常用的異丙醇-乙腈-甲醇-水,異丙醇-乙腈流動(dòng)相,在考察甲酸、乙酸、甲酸銨、乙酸銨、甲酸丁胺、甲酸二丁胺、甲酸三乙胺、甲酸二乙胺、甲酸甲胺、甲酸乙胺等不同電離增強(qiáng)劑的基礎(chǔ)上,比較了甲酸甲胺和常用的甲酸銨電離增強(qiáng)劑對(duì)LC-ESI-MS分析甘油三酯檢測(cè)靈敏度的影響,結(jié)果表明,甲酸甲胺可以使其中三亞油酸甘油酯組分的質(zhì)譜峰響應(yīng)值和信噪比均約為使用甲酸銨的5倍。考察了使用甲酸甲胺時(shí),甲酸甲胺電離增強(qiáng)劑的濃度、流動(dòng)相流速以及霧化氣流速對(duì)檢測(cè)的影響。通過(guò)測(cè)定不同玉米油濃度與其中甘油三酯總離子流色譜峰面積的關(guān)系曲線,顯示玉米油中甘油三酯組分在不同流動(dòng)相的電噴霧過(guò)程中出現(xiàn)聚集的最小濃度相差不大,三亞油酸甘油酯峰面積與濃度在7×10~(-7)~2×10~(-4)mol/L范圍內(nèi)的線性關(guān)系較好,相關(guān)系數(shù)R~2=0.9997,在更高的濃度時(shí)則峰面積增加緩慢。根據(jù)實(shí)驗(yàn)數(shù)據(jù)分析甲酸甲胺改進(jìn)檢測(cè)的機(jī)理,提出含有疏水性基團(tuán)的加合甲胺單電荷離子具有較低的溶劑化能,在霧滴表面富集的加合甲胺離子容易被蒸發(fā),從而提高了電噴霧離子化效率。本方法為L(zhǎng)C-ESIMS分析食用油中甘油三酯時(shí)提高檢測(cè)靈敏度提供了有效途徑。
[Abstract]:A method for improving the sensitivity of triglycerides by reversed phase liquid chromatography-electrospray mass spectrometry (LC-ESI-MS) using methylamine formate as a new ionization enhancer is proposed. Using reversed phase C _ (18) column and isopropanol solution of corn oil as the sample, the mobile phase of isopropanol-acetonitrile-methanol-water, isopropanol-acetonitrile, isopropanol-acetonitrile was selected, and the formic acid, acetic acid, ammonium formate, ammonium acetate and butylamine formate were investigated. On the basis of different ionization intensifiers such as dibutylamine formate, triethylamine formate, diethylamine formate, methylamine formate and ethylamine formate, the effects of methylamine formate and common ammonium formate ionization intensifier on the sensitivity of LC-ESI-MS determination of triglycerides were compared. The results show that the peak response and signal-to-noise ratio of trioleic acid glycerides are about 5 times as much as those of ammonium formate. The effects of the concentration of methylamine formate ionization enhancer, the mobile phase flow rate and the atomization flow rate on the determination of methylamine formate were investigated. By measuring the relationship between the concentration of different corn oil and the peak area of triglyceride total ion flow chromatography, it was found that the minimum concentration of triglyceride in corn oil showed little difference in the electrospray process of different mobile phases. The linear relationship between the peak area and concentration in the range of 7 脳 10 ~ (-7) ~ 2 脳 10 ~ (-4) mol/L was good, the correlation coefficient was 0.9997, and the peak area increased slowly at higher concentration. According to the experimental data, the mechanism of improving the detection of methylamine formate was analyzed. It was suggested that the adductive methylamine ion containing hydrophobic group had low solvation energy, and that the adductive methylamine ion enriched on the surface of droplet was easily evaporated. Thus, the efficiency of electrospray ionization is improved. This method provides an effective way to improve the detection sensitivity of triglycerides in edible oil by LC-ESIMS.
【作者單位】： 上海應(yīng)用技術(shù)大學(xué)化學(xué)與環(huán)境工程學(xué)院;
【基金】：國(guó)家自然科學(xué)基金(No.31671928) 上海市自然科學(xué)基金(No.15ZR1440800)資助項(xiàng)目~~
【分類號(hào)】：O657.63;TS227

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