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Electrospray ionization-quadrupole-time-of-flight mass spectrometry analyzing method of sterol contained in edible oil

An electrospray ionization and time-of-flight technology, applied in the field of mass spectrometry, can solve problems such as the difficulty of Coulomb explosion and ionization, the inability to meet high-throughput screening, and the difficulty of detecting animal sterols, etc., to improve reliability and accuracy , simple structure, and the effect of improving ionization efficiency

Inactive Publication Date: 2013-03-13
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the analysis methods of sterols in edible oil are mainly high-performance liquid chromatography-mass spectrometry (LC-MS) and gas chromatography-mass spectrometry (GC-MS), but the pretreatment is more complicated, and separation and purification processes such as thin-layer chromatography, ultra- Critical fluid extraction, solid phase extraction, etc., cannot meet the needs of high-throughput screening (J Am Oil Chem Soc 2009,86:1047–1055, Commun.Mass Spectrom.2006,20:2433–2440, Analytical Letters,2009,42 :1650-1661, Food Chemistry 2007, 102, 593–598)
[0004] In addition, sterol compounds are not easy to ionize due to their weaker proton affinity and weaker acidity, and the matrix of oil droplets is extremely complex, so they are easy to be wrapped in oil droplets, so it is difficult to cause Coulomb explosion and ionization, and the signal in ESI is weak , low sensitivity, and easily inhibited by other easily ionized substances, it is difficult to detect trace amounts of animal sterols in edible oils, especially when qualified edible oils are mixed with a small amount of inferior oils, it is even more difficult to detect
These limitations have prompted the development and application of new analytical methods

Method used

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  • Electrospray ionization-quadrupole-time-of-flight mass spectrometry analyzing method of sterol contained in edible oil
  • Electrospray ionization-quadrupole-time-of-flight mass spectrometry analyzing method of sterol contained in edible oil
  • Electrospray ionization-quadrupole-time-of-flight mass spectrometry analyzing method of sterol contained in edible oil

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Experimental program
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Effect test

Embodiment 1

[0045] Embodiment 1: Qualitative analysis of sterols in edible oil

[0046] The operation steps are as follows:

[0047] Divide edible oil (olive oil, salad oil, vegetable oil, gutter oil of unknown origin, and the mixture of these edible oils) into two equal parts, add 1-2mL potassium hydroxide: ethanol (volume ratio 1:1), 60- Saponify and hydrolyze at 70°C for 1-2h, add 2.5-5mL ether to extract twice, add water to wash the organic layer, add KOH to dry after combining the organic layer, blow dry with nitrogen; add 50-100μL 10-40% of the first sample Pyridine dichloromethane solution, then mixed with 50-100μL 10-40% trifluoromethanesulfonic anhydride dichloromethane for 5-20 minutes, add 50-100μL 10-40% deuterated pyridine dichloromethane to the second sample Solution, and then mixed with 50-100μL 10-40% trifluoromethanesulfonic anhydride dichloromethane for 5-20 minutes; the two reaction solutions were mixed and then diluted with methanol, injected 0.5-5μL, quadrupole-time ...

Embodiment 2

[0052] Embodiment 2: Quantitative analysis of sterols in edible oil

[0053] The quantitative analysis of edible oil sample, through the following steps: edible oil sample (olive oil, salad oil, waste oil of unknown origin, and the mixture of these edible oils) reacts with pyridine, the standard solution of identical volume is with same operating procedure and Deuterated pyridine reaction; two reaction solutions were mixed for electrospray ionization-quadrupole-time-of-flight tandem mass spectrometry analysis. The content of the target compound in the sample is calculated by comparing d 0 / d 5 The peak intensity and standard content of the peak pair are obtained, that is, calculated by the following formula: C 样品 is the content of the analyte in edible oil, C 标液 is the standard content, V 标液 is the volume of the standard solution, V 样品 is the volume of edible oil sample, I 0 is the peak intensity of the product obtained after derivatization of the sterol compound in th...

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Abstract

The invention relates to an ESI-Q-TOF MS (Electrospray Ionization-Quadrupole-Time-of-Flight Mass Spectrometry) analyzing method of an edible oil sample, and particularly relates to a method for qualitatively or quantitatively analyzing the sterols compounds contained in the edible oil sample by combining an N-alkyl pyridine isotope derivatization method with ESI-Q-TOF MS analysis. The method comprises the following steps of: carrying out sample pretreatment on a target analyte; reacting the alcoholic hydroxyl of the target analyte with pyridine or deuterated pyridine; and diluting a marked sample solution for the ESI-Q-TOF MS analysis. The method disclosed by the invention has the advantages of fastness, high efficiency and flexibility and lays a foundation for further measuring and identifying possible unqualified edible oil by identifying phytosterin and zoosterol which are contained in edible oil.

Description

technical field [0001] The invention relates to an analysis method of electrospray ionization-quadrupole-time-of-flight tandem mass spectrometry (ESI-Q-TOF MS) for sterols in edible oil samples, and furthermore, it is a combination of N-alkylpyridine isotope derivatization methods Electrospray ionization-quadrupole-time-of-flight tandem mass spectrometry (ESI-Q-TOF MS) is a method for the qualitative or quantitative analysis of sterols, including phytosterols and zoosterols, in edible oil samples. The analytical method is fast, efficient and sensitive. Due to repeated use, waste oil and other recycled low-quality oils often contain more animal-derived sterols. Therefore, by distinguishing phytosterols and animal sterols in edible oils, this method is used to further determine and distinguish possible waste oil and Other recycled low-quality oil lays the foundation. technical background [0002] The quality and safety of edible oil has become a concern of the whole society....

Claims

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Application Information

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IPC IPC(8): G01N27/62G01N27/626
Inventor 郭寅龙汪航张立张菁王昊阳贺小双陆森森
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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