【摘要】：提出使用甲酸甲胺作為新型電離增強劑改善反相液相色譜-電噴霧質譜(LC-ESI-MS)檢測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,選擇文獻中常用的異丙醇-乙腈-甲醇-水,異丙醇-乙腈流動相,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劑的基礎上,比較了甲酸甲胺和常用的甲酸銨電離增強劑對LC-ESI-MS分析甘油三酯檢測靈敏度的影響,結果表明,甲酸甲胺可以使其中三亞油酸甘油酯組分的質譜峰響應值和信噪比均約為使用甲酸銨的5倍�？疾炝耸褂眉姿峒装窌r,甲酸甲胺電離增強劑的濃度、流動相流速以及霧化氣流速對檢測的影響。通過測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系曲線,顯示玉米油中甘油三酯組分在不同流動相的電噴霧過程中出現(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范圍內的線性關系較好,相關系數(shù)R~2=0.9997,在更高的濃度時則峰面積增加緩慢。根據(jù)實驗數(shù)據(jù)分析甲酸甲胺改進檢測的機理,提出含有疏水性基團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LC-ESIMS分析食用油中甘油三酯時提高檢測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】： 上海應用技術大學化學與環(huán)境工程學院;
【基金】：國家自然科學基金(No.31671928) 上海市自然科學基金(No.15ZR1440800)資助項目~~
【分類號】：O657.63;TS227

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