Pretreatment method for essence gas chromatography-mass spectrometry combination detection
A gas chromatography-mass spectrometry and essence technology, which is applied in the pretreatment field of ultrasonic-assisted dispersion liquid-phase microextraction, can solve the problems of reduced operation steps, high cost, easy loss of aroma, etc., and achieves the effect of easy operation, simple method and good effect
Inactive Publication Date: 2013-08-07
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 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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[0017] A pretreatment method for ultrasonic-assisted dispersion liquid-phase microextraction for the detection of essence by gas chromatography-mass spectrometry, comprising the following steps: taking 0.5g of essence sample in a 50mL centrifuge tube, and mixing carbon tetrachloride (dispersant) and acetone ( Extraction agent) according to the ratio of 1:10 to mix evenly to obtain a mixed solution, absorb the mixed solution and pour it into the bottom of the centrifuge tube to form a uniform emulsion, after ultrasonic cleaning for 10 minutes, place it on a vortex mixer and shake for 20 minutes After taking it out, centrifuge it for 10min, remove the supernatant liquid, dry it, add acetone to make it to 1mL, and then analyze it in the instrument.
[0018] Fragrance aroma analysis method: GC-MS analysis
[0019] Gas chromatography conditions: HB-5 capillary column (30m×0.25μm×0.25μm), the temperature of the injection port is 250°C, the carrier gas is high-purity (≥99.999%) heliu...
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The invention relates to a pretreatment method for essence gas chromatography-mass spectrometry combination detection. The pretreatment method comprises the following steps: taking an essence sample, placing the sample into a 50 mL centrifuge tube, uniformly mixing carbon tetrachloride and acetone to obtain a mixing solution, sucking the mixing solution, injecting from the bottom of the centrifuge tube to form a uniform emulsion, carrying out ultrasound on an ultrasonic cleaning device, placing on a vortex mixer to shock, taking, carrying out centrifugation, removing the lower layer supernatant, carrying out blow-drying, adding acetone, carrying out volume metering to achieve a volume of 1 mL, and adding to an instrumental to analyze. The pretreatment method has characteristics of simpleness, easy operation, short time and good effect.
Description
technical field [0001] The invention relates to a pretreatment method for essence detection, in particular to an ultrasonic-assisted dispersion liquid phase microextraction pretreatment method for essence gas chromatography mass spectrometry detection. 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 the...
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IPC IPC(8): G01N30/06
Inventor 刘娜
Owner TIANJIN CHUNFA BIO TECH GRP