CN104730176A - Analysis detection method for determining 3-methylmercapto-propionaldehyde - Google Patents

Abstract

The invention relates to an analysis detection method for determining 3-methylmercapto-propionaldehyde. The analysis detection method comprises the following steps: (1) accurately weighing 0.1g of powder containing the 3-methylmercapto-propionaldehyde, putting the powder into a 5mL centrifugal tube, sucking 1mL of distilled water by using a pipettor to dissolve the powder, after the powder is completely dissolved, adding 2mL of diethyl ether into a vortex shaking device to for shaking for 30 seconds, standing, layering, sucking 1mL of liquid supernatant, adding anhydrous sodium sulfate into the 1mL of liquid supernatant, shaking, and filtering with a film to obtain a solution to be detected; and (2) putting the solution to be detected in the step (1) into a dry head-space bottle, screwing a sealing cover, pre-heating at a pre-set sampling temperature for 10 minutes, adsorbing and sampling by an extraction head, wherein the sampling temperature is 100 DEG C and the sampling time is 51 minutes, injecting the solution into a GC-MS to be detected, and resolving for 5 minutes. The SPME-GC-MS method has high precision of a detection result and good reliability.

Description

A kind of analyzing detecting method measuring 3-methylthiopropionaldehyde

Technical field

The present invention relates to a kind of detection method, particularly a kind of analyzing detecting method measuring 3-methylthiopropionaldehyde.

Background technology

3-methylthiopropionaldehyde is kind of a colourless or flaxen liquid, and density is a bit larger tham water, and boiling point is higher, reaches 165 DEG C, water insoluble, is dissolved in ethanol, propylene glycol and oils.There is the odor characteristic that mellow sauce is fragrant, onion is fragrant and pork braised in brown sauce is fragrant, national regulations its be the food spices allowing use, be mainly used in baked goods, flavouring, soft drink and candy.

The volatile ingredient of solid-phase microextraction (SPME) directly above collection liquid or solid material, complicated sample matrices composition is made to be brought into the possibility of analytical instrument system together when liquid or solid can be avoided to sample, thus elimination matrix composition and solvent detect the impact and interference that cause on sample volatile ingredient, be highly suitable for the research of volatile matter.

Summary of the invention

The object of this invention is to provide a kind of analyzing detecting method measuring 3-methylthiopropionaldehyde.

The technical solution used in the present invention is:

Measure an analyzing detecting method for 3-methylthiopropionaldehyde, comprise the steps:

(1) extraction of 3-methylthiopropionaldehyde:

Accurately take 0.1g contain the powder of 3-methylthiopropionaldehyde and be placed in the centrifuge tube of 5mL, draw 1ml distilled water with pipettor afterwards to be dissolved, dissolve completely until it, the ether adding 2mL is placed in turbula shaker and vibrates 30s, stratification, Aspirate supernatant 1mL, and add anhydrous sodium sulfate vibration, cross film (organic filter membrane of 0.22um), be liquid to be measured;

(2) GC-MS of 3-methylthiopropionaldehyde detects

The liquid to be measured of step (1) gained is placed in dry ml headspace bottle, screwing hermetic lid, under the sample temperature of setting after preheating 10min, extracting head adsorption sampling, sample temperature 100 DEG C, sampling time 51min, reinject in GC-MS and detect, resolve 5min.

Preferably, in described step (2), extracting head model is 50/30 μm of DVB/CAR/PDMS extracting fiber.

Preferably, described GC-MS condition is:

Chromatographic column: DB-5ms 0.25mm × 30m × 0.25 μm;

Chromatographic condition: injector temperature: 260 DEG C, carrier gas: He, flow: l.2mL/min;

Heating schedule: initial temperature 37 DEG C, keeps 2min, rises to 180 DEG C, then rise to 210 DEG C with 15 DEG C/min with 0.5 DEG C/min, keeps 2min;

Mass Spectrometry Conditions: ionization mode: EI, ion source temperature 230 DEG C, electron energy 70e V, mass scan range: 10m/z-800m/z.

The beneficial effect that the present invention has:

Solid-phase microextraction extraction method of the present invention can avoid the interference of matrix composition and solvent, has certain advantage in the context of detection of volatile ingredient.SPME-GC-MS method testing result precision is high, good reliability.

Embodiment

Below in conjunction with specific embodiment, the invention will be further described, but do not limit protection scope of the present invention.

Embodiment 1

Measure an analyzing detecting method for 3-methylthiopropionaldehyde in essence powder, comprise the steps:

(1) extraction of 3-methylthiopropionaldehyde

Accurately take the powdered flavor that 0.1g contains 3-methylthiopropionaldehyde, put into the centrifuge tube of 5mL, draw 1ml distilled water with pipettor afterwards to be dissolved, dissolve completely until it, the ether adding 2mL is placed in turbula shaker and vibrates 30s, stratification, Aspirate supernatant 1mL, and add the vibration of 0.5g anhydrous sodium sulfate, cross film (organic filter membrane of 0.22um), be liquid to be measured;

(2) GC-MS of 3-methylthiopropionaldehyde detects

Liquid to be measured in step (1) is placed in dry ml headspace bottle, screwing hermetic lid, under the sample temperature of setting after preheating 10min, extracting head adsorption sampling, sample temperature 100 DEG C, sampling time 51min, reinject in GC-MS and detect, resolve 5min;

Extracting head model: 50/30 μm of DVB/CAR/PDMS extracting fiber;

Described GC-MS condition is:

Chromatographic column: DB-5ms 0.25mm × 30m × 0.25 μm;

Chromatographic condition: injector temperature: 260 DEG C, carrier gas: He, flow: l.2mL/min;

Heating schedule: initial temperature 37 DEG C, keeps 2min, rises to 180 DEG C, then rise to 210 DEG C with 15 DEG C/min with 0.5 DEG C/min, keeps 2min.

Mass Spectrometry Conditions: ionization mode: EI, ion source temperature 230 DEG C, electron energy 70e V, mass scan range: 10m/z ~ 800m/z.

Claims (3)

1. measure an analyzing detecting method for 3-methylthiopropionaldehyde, it is characterized in that: comprise the steps:

(1) extraction of 3-methylthiopropionaldehyde:

Accurately take 0.1g contain the powder of 3-methylthiopropionaldehyde and be placed in the centrifuge tube of 5mL, draw 1ml distilled water with pipettor afterwards to be dissolved, dissolve completely until it, the ether adding 2mL is placed in turbula shaker and vibrates 30s, stratification, Aspirate supernatant 1mL, and add anhydrous sodium sulfate vibration, cross film (organic filter membrane of 0.22um), be liquid to be measured;

(2) GC-MS of 3-methylthiopropionaldehyde detects

The liquid to be measured of step (1) gained is placed in dry ml headspace bottle, screwing hermetic lid, under the sample temperature of setting after preheating 10min, extracting head adsorption sampling, sample temperature 100 DEG C, sampling time 51min, reinject in GC-MS and detect, resolve 5min.

2. a kind of analyzing detecting method measuring 3-methylthiopropionaldehyde according to claim 1, is characterized in that: in described step (2), extracting head model is 50/30 μm of DVB/CAR/PDMS extracting fiber.

3. a kind of analyzing detecting method measuring 3-methylthiopropionaldehyde according to claim 1 or 2, is characterized in that: described GC-MS condition is:

Chromatographic column: DB-5ms 0.25mm × 30m × 0.25 μm;

Chromatographic condition: injector temperature: 260 DEG C, carrier gas: He, flow: l.2mL/min;

Heating schedule: initial temperature 37 DEG C, keeps 2min, rises to 180 DEG C, then rise to 210 DEG C with 15 DEG C/min with 0.5 DEG C/min, keeps 2min;

Mass Spectrometry Conditions: ionization mode: EI, ion source temperature 230 DEG C, electron energy 70e V, mass scan range: 10m/z-800m/z.