Pretreatment method for combined detecting on gas chromatograph and mass spectrum of powdered essence

A gas chromatography-mass spectrometry and essence technology, which is applied in the pretreatment field of reverse solid-phase matrix dispersion purification, can solve the problems of many artificial effects, distortion of the aroma of the analysis liquid, and reduction of operation steps, so as to improve the test efficiency, good reproducibility, easy-to-handle effects

Active Publication Date: 2012-09-26
TIANJIN CHUNFA BIO TECH GRP
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Problems solved by technology

Simultaneous distillation and extraction is a method of extracting volatile components developed by Nickeron and Likens in 1966. The device integrates extraction, distillation, extraction and concentration, which reduces the number of operating steps, is simple to operate, and has high extraction efficiency; The obvious disadvantage is that there are many artificial effects produced by long-term high-temperature cooking, and the obtained analytical solution has obvious aroma distortion.
Liquid-liquid extraction belongs to the classic solvent extraction separation technology. It is a method of purifying and extracting by using the solubility diffe

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  • Pretreatment method for combined detecting on gas chromatograph and mass spectrum of powdered essence
  • Pretreatment method for combined detecting on gas chromatograph and mass spectrum of powdered essence
  • Pretreatment method for combined detecting on gas chromatograph and mass spectrum of powdered essence

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Embodiment 1

[0020] A reverse solid-phase matrix dispersion purification pretreatment method for detection of powdered flavor by gas chromatography-mass spectrometry, comprising the following steps: after pulverizing and drying the powdery flavor sample, weighing 10 g of the flavor sample into a 50 mL stoppered centrifuge test tube, Add 20g of anhydrous sodium sulfate and vortex stir, after mixing evenly, add 20mL of acetone / n-hexane (v:v=1:1) extract, vortex mix for 2min, then ultrasonically extract for 5min, repeat twice, centrifuge at 3000r / min After removing suspended particles for 10 minutes, take 1 mL of the supernatant in a centrifuge tube, add 50 mg of PSA and 100 mg of anhydrous magnesium sulfate for purification, vortex and mix for 2 minutes, then ultrasonically extract for 5 minutes, then centrifuge at 3000 r / min for 5 minutes, and take 1 μL of the supernatant The fragrance composition was analyzed by gas chromatography-mass spectrometry (GC-MS). GC-MS analysis conditions are: ...

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Abstract

The invention relates to a pretreatment method for combined detecting on gas chromatograph and mass spectrum of a powdered essence. The method is characterized by comprising the following steps of: after crushing and drying a powdered essence sample, weighing the essence sample into a 50 mL centrifuge tube with a plug, adding anhydrous sodium sulfate into the tube to be vortex stirred and mixed evenly, adding an acetone/n-hexane extracting solution, vortex stirring and ultrasonically extracting twice, centrifuging to remove suspended particles, taking the supernatant liquor into a centrifuge tube, adding phenolsulfonic acid (PSA) and anhydrous magnesium sulfate to carry out purifying treatment, vortex mixing and ultrasonically extracting, and centrifuging to take the supernatant liquor, so that a liquor to be detected which is used for detecting the ingredients of the essence by a gas Chromatography and mass spectrometer is obtained. The sample pretreatment method adopted by the invention is easy to operate, short in time and good in reproducibility, and can obviously improve the experiment efficiency.

Description

technical field [0001] The invention relates to the detection technology of powdery essence, in particular to a reverse solid-phase matrix dispersion purification pretreatment method for detection of powdery essence by gas chromatography-mass spectrometry. Background technique [0002] At present, the commonly used pretreatment methods mainly include the following: Solid-phase microextraction is a sample pre-separation and enrichment method developed in the 1990s. It integrates sample pretreatment and sample injection, and purifies the sample. , After enrichment, it can be combined with various analysis methods and is especially suitable for the analysis and determination of organic matter. However, SPME also has certain shortcomings. The fused silica fiber is very fragile and easy to break, so it must be handled with great care. The volume of the fiber stationary phase is small, the absolute quality of the aroma of the adsorbed phase is very limited, the detection limit of...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/14
Inventor 刘娜
Owner TIANJIN CHUNFA BIO TECH GRP
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