Method for qualitative and quantitative determination of sugar alcohols in foods by ion chromatograph-mass spectrometer

A technology of ion chromatography and quantitative determination, which is applied in the field of analysis of sugar alcohol components, can solve the problems of time-consuming, etc., and achieve the effects of avoiding false positives, reducing costs, and having little matrix interference

Active Publication Date: 2013-10-09
镇江出入境检验检疫局检验检疫综合技术中心
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  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

The method used in conditional gas chromatography-mass spectrometry requires the sample to be derivatized, reconstituted by nitrogen blowing, and then injected, which takes a long time

Method used

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  • Method for qualitative and quantitative determination of sugar alcohols in foods by ion chromatograph-mass spectrometer
  • Method for qualitative and quantitative determination of sugar alcohols in foods by ion chromatograph-mass spectrometer
  • Method for qualitative and quantitative determination of sugar alcohols in foods by ion chromatograph-mass spectrometer

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Experimental program
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Effect test

Embodiment 1

[0044] Sample pretreatment:

[0045] Take 0.5g sample of German chocolate biscuit in a 50mL centrifuge tube, add 25mL water, vortex mix for 3 minutes, and ultrasonically extract for 10min. Take 5mL of the supernatant in a 10mL centrifuge tube, add 5mL of n-hexane to vortex mix, centrifuge at 5000 rpm for 10min, remove the n-hexane layer, take 2mL of the lower layer into another centrifuge tube, add 3mL of acetonitrile to vortex, and place in a refrigerated centrifuge Refrigerate and centrifuge at 5000 rpm for 15 min at -15°C, take 1.5 mL of the supernatant, put it in another test tube, dry it with nitrogen, add 3.5 mL of water to reconstitute, vortex, and pass through the aqueous phase membrane and SPE column. 25.0 μL of the filtrate was taken for ICS-MS detection, and the detection conditions of ICS-MS were the same as those of the ion chromatography mass spectrometry detection conditions of the above-mentioned standard mixed working solution, and the qualitative and quantita...

Embodiment 2

[0047] Taking China Mirin as the sample, take 0.2g sample and add water to a 100mL volumetric flask to make up to volume, pass through the aqueous phase membrane and SPE column, and the filtrate is used for ICS-MS detection. 25.0 μL of the filtrate was taken for ICS-MS detection. The detection conditions of ICS-MS were the same as those of the ion chromatography-mass spectrometry detection conditions of the above standard mixed working solution. The qualitative and quantitative analysis of the six sugar alcohols was carried out.

Embodiment 3

[0049] Take Indonesian ginger candy as a sample, take 0.8g sample in a mortar, add a small amount of water to fully grind it, transfer it to a 100mL volumetric flask, add water to make up to the mark. Take 10 mL of the solution and centrifuge at -15 °C at 5000 rpm for 15 min in a refrigerated centrifuge, take 5 mL of the supernatant to pass through the aqueous phase membrane and SPE column, and the filtrate is used for ICS-MS detection. 25.0 μL of the filtrate was taken for ICS-MS detection, and the detection conditions of ICS-MS were the same as those of the ion chromatography mass spectrometry detection conditions of the above-mentioned standard mixed working solution, and the qualitative and quantitative analysis of the six sugar alcohols was carried out.

[0050] The samples were analyzed under the same ICS-MS ion chromatography-mass spectrometry conditions as the detection standard mixed working solution, and a method for the detection of sugar alcohols in food by ion ch...

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PUM

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Abstract

The invention discloses a method for qualitative and quantitative determination of sugar alcohols in foods by an ion chromatograph-mass spectrometer. The method is characterized in that a sample subjected to extraction purification pre-treatment is detected by the ion chromatograph-mass spectrometer; ion chromatography conditions comprise that 90mmoL/L of a sodium hydroxide solution as a separation column eluting solution is used for isocratic elution at a flow rate of 0.50mL/min; a suppressed conductance method comprising a suppressor electric current of 139mA, a feeding amount of 25.0 microliters and a suppressor water source constant flow pump flow rate of 1.0mL/min is adopted; mass spectrometry conditions comprise that an ionization mode APCI- is adopted and a temperature of fainting during acupuncture treatment is 450 DEG C; atomized gas is nitrogen and has purity of 99.9% and pressure of 55psi; and quantitative analysis adopts an external standard quantitative method. The method realizes on-line qualitative and quantitative detection of sugar alcohols in foods, utilizes a self-made SPE column and the ion chromatograph-mass spectrometer to carry out detection, and realizes simple and fast qualitative and quantitative detection of six sugar alcohols in foods.

Description

technical field [0001] The invention relates to the field of detection and analysis in the field of food, in particular to an analysis method for sugar alcohol components in food. Background technique [0002] In the inspection and quarantine department, it is necessary to conduct qualitative and quantitative detection of the sugar alcohol content of food, but the current detection methods have some defects. At present, the detection methods of sugar alcohols in food at home and abroad include: high performance liquid chromatography - evaporative light scattering method, high performance liquid chromatography - differential refraction detection method, ion exclusion liquid chromatography, gas chromatography, gas chromatography mass spectrometry, liquid phase chromatography tandem mass spectrometry, etc. Evaporative light scattering, differential refraction detection, ion exclusion liquid chromatography, gas chromatography, etc. cannot meet the requirements of EU Directive 6...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 周洪斌
Owner 镇江出入境检验检疫局检验检疫综合技术中心
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