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

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...

AI Technical Summary

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 difference between the component to be tested and the sample matrix in the two immiscible phases, but the aroma is easily lost during the operation.

Solid-phase extraction is a kind of adsorbent extraction. The sample passes through a disposable extraction column filled with adsorbent. The analyte and impurities are retained on the column, and then the impurities are removed with a selective solvent to elute the analyte, so as to achieve the separation. Purpose; the disadvantage is that the cost is high, and there is a certain difficulty in the selection of fillers and eluents, which is more suitable for pretreatment experiments of specific substances

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