Establishing method for high-resolution mass spectrum database of anti-oxidants and antiseptic, and detection method for anti-oxidants and antiseptic

A high-resolution mass spectrometry and antioxidant technology, which is applied in the detection of antioxidants and preservatives, can solve the problem of lack of secondary spectrum databases, no further discussion on the influencing factors of high-resolution mass spectrometry screening targets, and lack of secondary spectrum data information. question

Active Publication Date: 2016-09-07
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Abstract
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Problems solved by technology

Regarding the analysis of antioxidants and preservatives in vegetable oils, the method used a reversed-phase C18 column and quantitatively analyzed 11 target substances in negative ion mode, but the influencing factors of high-resolution mass spectrometry screening targets were not further discussed
[0005] Moreover, there are many general-purpose primary mass spectrometry databases at present, but very few publicly available secondary mass spectrometry databases, especially for certain specific analysis and monitoring ranges. If a corresponding secondary mass spectrometry database is established, the analysis target confirm the results of
In the target analysis of known targets, you can search in many chemical substance structure databases to obtain information such as compound names, molecular formulas and structures, such as PUBCHEM, ChemSpider, ChEBI, etc., but the secondary spectrum data information is only available in MASSBANK.

Method used

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  • Establishing method for high-resolution mass spectrum database of anti-oxidants and antiseptic, and detection method for anti-oxidants and antiseptic
  • Establishing method for high-resolution mass spectrum database of anti-oxidants and antiseptic, and detection method for anti-oxidants and antiseptic
  • Establishing method for high-resolution mass spectrum database of anti-oxidants and antiseptic, and detection method for anti-oxidants and antiseptic

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Embodiment 1

[0116] 1.1 Standard solution preparation

[0117] Standard solution: Weigh 7.5-10.0mg of the standard product, dilute it to a 25mL volumetric flask with methanol, and prepare a 0.3-0.4mg / mL single-standard methanol solution; pipette 25-35μL of the single-standard methanol solution, and use Dilute methanol to a 10mL volumetric flask, prepare a single standard methanol solution of about 1.0μg / mL, and refrigerate at 4°C until use.

[0118] 1.2 Mass Spectrometry Conditions

[0119] Electrospray ESI ion source: positive ion full scan mode, capillary voltage: 3500V; atomizing gas: 1.5Bar; drying gas temperature: 180°C; drying gas flow rate: 6.0l / min; mass scanning range: m / z 50-1000amu ; Hexapod RF voltage: 200.0Vpp; Collision cell RF voltage: 600.0Vpp.

[0120] Negative ion full scan mode; capillary voltage: 3000V; atomizing gas: 1.5Bar; drying gas temperature: 180°C; drying gas flow rate: 6.0l / min; mass scanning range: m / z 50-1000amu; quadrupole ion energy: 4.0eV; collision cel...

Embodiment 2

[0126] 2.1 Standard solution preparation

[0127] Standard stock solution: Weigh 7.5-10.0 mg of standard product, dilute to 25 mL volumetric flask with methanol, and prepare 0.3-0.4 mg / mL single-standard methanol solution; pipette 25-35 μL single-standard methanol solution, Dilute to a 10mL volumetric flask with methanol, prepare a single standard methanol solution of about 1.0μg / mL, and refrigerate at 4°C until use.

[0128] Single standard working solution: dilute 1.0μg / mL single standard by 1 time (about 500ppb single standard); mixed standard working solution: pipette 15-20μL 0.3-0.4mg / mL single standard methanol solution to 10mL In the volumetric flask, use methanol to make up the volume (about 500ppb mixed standard). Refrigerate at 4°C until use.

[0129] 2.2 Chromatographic conditions

[0130] High performance liquid chromatography conditions: Luna C8 liquid chromatography column (4.6 mm×3 μm×150 mm, Phenomenex Company).

[0131] Mobile phase A is formic acid water ...

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Abstract

The invention provides an establishing method for a high-resolution mass spectrum database of anti-oxidants and antiseptic, and a detection method for anti-oxidants and antiseptic. The detection method comprises the following steps: respectively preparing single-standard methanol solutions of anti-oxidants and antiseptic and carrying out mass spectrometry with a time-of-flight mass spectrometer in a positive ion full scanning mode and a negative ion full scanning mode so as to establish the high-resolution mass spectrum database; and extracting a to-be-detected sample with alcoholic solutions, carrying out mass spectrometry and detecting the anti-oxidants and antiseptic in the sample according to mass spectral data and the high-resolution mass spectrum database. Compared with the prior art, the invention has the advantages that since high-resolution mass spectrum and target analysis strategies are employed for detection of the anti-oxidants and antiseptic, the method can carry out rapid qualitative detection on a plurality of anti-oxidants and antiseptic at the same time without complex pre-treatment steps; a combination of liquid chromatography and high0resolution mass spectrometry is employed, so the method is high in accuracy and sensitivity; and the method can carry out qualitative determination on screened unknown anti-oxidants and antiseptic, so the scope of analysis and monitoring is broadened.

Description

technical field [0001] The invention belongs to the technical field of chemical detection, and in particular relates to a method for establishing a high-resolution mass spectrum database of antioxidants and preservatives and a method for detecting antioxidants and preservatives. Background technique [0002] Compared with the 2011 edition of my country's National Food Safety Standard GB 2760 "Use of Food Additives" in 2014, 27 kinds of tea polyphenol palmitate were added to the list of antioxidants, and 4-phenylphenol, 2- Phenylphenol sodium salt, ethyl naphthol and sec-butylamine, added ε-polylysine, hydrochloride, lysozyme, two versions with a total of 30 preservatives. In the face of so many additives, how to quickly screen the information of multiple additives has always been a hot spot in the field of safety and supervision. [0003] The implementation of tobacco control has brought about new changes in tobacco consumption. The sales of non-combustible tobacco products,...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72G01N2030/027
Inventor 刘彤陈欢韩书磊付亚宁张小涛刘洋
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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