CN105004818A - Detection method for plasticizers in foods containing oils and fats - Google Patents

Abstract

The invention belongs to the technical field of food detection methods, and particularly relates to a detection method for plasticizers in foods containing oils and fats. Neutral alumina and acetonitrile are used for extracting the oils and fats in the foods containing the oils and fats, the method is simple and easy to implement, pretreatment time is greatly shortened, and the pretreatment cost is greatly lowered. In the extraction process of sixteen kinds of plasticizers, the fats do not need to be extracted, the extracting agent acetonitrile in the vortex process can sufficiently make contact with a sample matrix, in this way, extracting is more sufficient and thorough, and the recovery rate of the plasticizers is greatly increased. In addition, in the pretreatment process, using of toxic and harmful reagents is reduced, harm to the environment and the human body is reduced in the detection process, and the detection method is environmentally friendlier compared with the prior art.

Description

A kind of detection method containing plasticiser in fatty foods

Technical field

The invention belongs to food detection method technical field, particularly relate to a kind of detection method containing plasticiser in fatty foods.

Background technology

Plasticiser, also known as plastifier, is the industrial macromolecular material auxiliary agent be widely used, has larger toxicity, belong to a kind of Environmental Hormone to human body.Plasticiser does not belong to food additives, do not allow to be added in food, but plasticiser is a kind of fat-soluble fabulous material, so plasticiser can migrate in food from food Package, especially enter in grease-contained food, therefore need by detecting the content determining plasticiser in food, thus guarantee the safety to human body.

The existing detection method containing plasticiser in fatty foods is, fatty foods sample sherwood oil extraction lubricant component wherein will be contained, grease extraction obtained mixes with ethyl acetate, cyclohexane (volume ratio 1:1) solution gets filtrate, filtrate is through gel permeation chromatography device (GPC) purified treatment, collect efflux, after reduced pressure concentration, chromatography of gases-GC-MS is adopted to detect the content of plasticiser in sample.

The shortcoming that above-mentioned detection method exists is: 1, will use a large amount of poisonous and harmful chemical reagent in oil extraction processes and plasticiser leaching process, especially GPC processing procedure, use a large amount of ethyl acetate and cyclohexane, comparatively major injury is all caused to laboratory operation personnel and environment; 2, GPC device is expensive, and processing speed slowly, and each sample needs about 40-60min, causes testing cost high, length consuming time; 3, sherwood oil extracts grease thoroughly, causes the detection recovery of plasticiser low.

Summary of the invention

The present invention is directed to the deficiency that above-mentioned prior art exists, provide a kind of efficient easily containing the detection method of plasticiser in fatty foods.

The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of detection method containing plasticiser in fatty foods, and step is as follows:

(1) extract, purify: what take even sample preparation is placed in color comparison tube containing fatty foods sample 1.0-3.0g, add neutral alumina aluminium powder 2.0-3.0g wherein, after vibration mixes, add 8-10ml acetonitrile, vortex 60-100s, the centrifugal 5min of 2500-3000r/min, gets upper strata acetonitrile extract, is placed in sample injection bottle to be detected;

(2) GC/MS detects:

A, chromatographic condition

Chromatographic column: HP-5MS quartz capillary column [30m × 0.25mm (internal diameter) × 0.25 μm];

Injector temperature: 250 DEG C;

Heating schedule: initial column temperature 60 DEG C, keeps 1min, is warming up to 220 DEG C with 20 DEG C/min, keeps 1min, then is warming up to 280 DEG C with 5 DEG C/min, keeps 4min;

Carrier gas: helium (purity >=99.999%), flow velocity 1ml/min;

Input mode: Splitless injecting samples;

Sample size: 1 μ L;

B, Mass Spectrometry Conditions

Chromatogram and mass spectrometer interface temperature: 280 DEG C;

Ionization mode: electron bombardment ionization source EI;

Detection mode: ion scan Mode S IM, detects ionic conditions:

Ionizing energy: 70eV;

Solvent delay: 5min.

The invention has the beneficial effects as follows: the present invention uses neutral alumina and acetonitrile to extract containing the grease in fatty foods, and method is simple, greatly reduces time and the cost of pre-treatment; In 16 kinds of plasticiser extraction processes, without the need to extracting fat, the extraction agent acetonitrile of vortex process can fully contact with sample substrate, extracts more fully thoroughly, improves the recovery of plasticiser largely.Decrease the use of poisonous and harmful reagent in addition in this method pretreatment process, reduce the harm of testing process to environment and human body, than prior art environmental protection more.

On the basis of technique scheme, the present invention can also do following improvement.

Further, described neutral alumina is for analyzing pure neutral alumina.

Further, described acetonitrile is HPLC level acetonitrile.

Accompanying drawing explanation

Fig. 1 is SIM chromatogram of the present invention.

Embodiment

Be described principle of the present invention and feature below in conjunction with example, example, only for explaining the present invention, is not intended to limit scope of the present invention.

The hybrid standard product solution of preparation containing 16 kinds of plasticisers, dibutyl phthalate DBP 200 μ g/kg is added in negative peanut oil, soybean oil, chilli oil, add phthalic acid (2-ethyl) own ester DEHP 500 μ g/kg, except above two kinds, the addition of other 14 kinds of plasticisers is 300 μ g/kg, Pitch-based sphere is equal to or is less than the limit standard of China, and each contents level repeats 4 times.

Embodiment 1

Get above-mentioned peanut oil, detect its content of plasticizing agent, step is as follows:

(1) extract, purify: what take even sample preparation is placed in 10ml color comparison tube containing fatty foods sample 1.0g, add neutral alumina aluminium powder 2.0g wherein, after vibration mixes, add 8ml acetonitrile, vortex 60s, the centrifugal 5min of 2500r/min, gets upper strata acetonitrile extract, is placed in sample injection bottle to be detected;

(2) GC/MS detects:

A, chromatographic condition

Chromatographic column: HP-5MS quartz capillary column [30m × 0.25mm (internal diameter) × 0.25 μm];

Injector temperature: 250 DEG C;

Heating schedule: initial column temperature 60 DEG C, keeps 1min, is warming up to 220 DEG C with 20 DEG C/min, keeps 1min, then is warming up to 280 DEG C with 5 DEG C/min, keeps 4min;

Carrier gas: helium (purity >=99.999%), flow velocity 1ml/min;

Input mode: Splitless injecting samples;

Sample size: 1 μ L;

B, Mass Spectrometry Conditions

Chromatogram and mass spectrometer interface temperature: 280 DEG C;

Ionization mode: electron bombardment ionization source EI;

Detection mode: ion scan Mode S IM, detects ionic conditions:

Ionizing energy: 70eV;

Solvent delay: 5min.

The average recovery rate of the content of plasticizing agent in the peanut oil obtained and relative standard deviation RSD are in table 1.

Embodiment 2

Get above-mentioned soybean oil, detect the content of its plasticiser, step is as follows:

(1) extract, purify: what take even sample preparation is placed in 10ml color comparison tube containing fatty foods sample 2.0g, add neutral alumina aluminium powder 2.5g wherein, after vibration mixes, add 10ml acetonitrile, vortex 100s, the centrifugal 5min of 3000r/min, gets upper strata acetonitrile extract, is placed in sample injection bottle to be detected;

(2) GC/MS detects:

A, chromatographic condition

Chromatographic column: HP-5MS quartz capillary column [30m × 0.25mm (internal diameter) × 0.25 μm];

Injector temperature: 250 DEG C;

Heating schedule: initial column temperature 60 DEG C, keeps 1min, is warming up to 220 DEG C with 20 DEG C/min, keeps 1min, then is warming up to 280 DEG C with 5 DEG C/min, keeps 4min;

Carrier gas: helium (purity >=99.999%), flow velocity 1ml/min;

Input mode: Splitless injecting samples;

Sample size: 1 μ L;

B, Mass Spectrometry Conditions

Chromatogram and mass spectrometer interface temperature: 280 DEG C;

Ionization mode: electron bombardment ionization source EI;

Detection mode: ion scan Mode S IM, detects ionic conditions:

Ionizing energy: 70eV;

Solvent delay: 5min.

The average recovery rate of the content of plasticizing agent in the soybean oil obtained and relative standard deviation RSD are in table 1.

Embodiment 3

Get above-mentioned chilli oil, detect the content of its plasticiser, step is as follows:

(1) extract, purify: what take even sample preparation is placed in 10ml color comparison tube containing fatty foods sample 3.0g, add neutral alumina aluminium powder 3.0g wherein, after vibration mixes, add 8ml acetonitrile, vortex 80s, the centrifugal 5min of 3000r/min, gets upper strata acetonitrile extract, is placed in sample injection bottle to be detected;

(2) GC/MS detects:

A, chromatographic condition

Chromatographic column: HP-5MS quartz capillary column [30m × 0.25mm (internal diameter) × 0.25 μm];

Injector temperature: 250 DEG C;

Heating schedule: initial column temperature 60 DEG C, keeps 1min, is warming up to 220 DEG C with 20 DEG C/min, keeps 1min, then is warming up to 280 DEG C with 5 DEG C/min, keeps 4min;

Carrier gas: helium (purity >=99.999%), flow velocity 1ml/min;

Input mode: Splitless injecting samples;

Sample size: 1 μ L;

B, Mass Spectrometry Conditions

Chromatogram and mass spectrometer interface temperature: 280 DEG C;

Ionization mode: electron bombardment ionization source EI;

Detection mode: ion scan Mode S IM, detects ionic conditions:

Ionizing energy: 70eV;

Solvent delay: 5min.

The average recovery rate of the content of plasticizing agent in the chilli oil obtained and relative standard deviation RSD are in table 1.

Table 1

As can be seen from data in table 1, respectively contain the average recovery rate of plasticiser in fatty foods all 80 ~ 120%, relative standard deviation RSD is all not more than 10%, and the recovery and relative standard deviation all meet plasticiser residue detection standard.

The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (3)

1., containing a detection method for plasticiser in fatty foods, it is characterized in that, step is as follows:

(1) extract, purify: what take even sample preparation is placed in color comparison tube containing fatty foods sample 1.0-3.0g, add neutral alumina aluminium powder 2.0-3.0g wherein, after vibration mixes, add 8-10ml acetonitrile, vortex 60-100s, the centrifugal 5min of 2500-3000r/min, gets upper strata acetonitrile extract, is placed in sample injection bottle to be detected;

(2) GC/MS detects:

A, chromatographic condition

Chromatographic column: HP-5MS quartz capillary column [30m × 0.25mm (internal diameter) × 0.25 μm];

Injector temperature: 250 DEG C;

Heating schedule: initial column temperature 60 DEG C, keeps 1min, is warming up to 220 DEG C with 20 DEG C/min, keeps 1min, then is warming up to 280 DEG C with 5 DEG C/min, keeps 4min;

Carrier gas: helium (purity >=99.999%), flow velocity 1ml/min;

Input mode: Splitless injecting samples;

Sample size: 1 μ L;

B, Mass Spectrometry Conditions

Chromatogram and mass spectrometer interface temperature: 280 DEG C;

Ionization mode: electron bombardment ionization source EI;

Detection mode: ion scan Mode S IM, detects ionic conditions:

Ionizing energy: 70eV;

Solvent delay: 5min.

2. detection method according to claim 1, is characterized in that, described neutral alumina is for analyzing pure neutral alumina.

3. detection method according to claim 1, is characterized in that, described acetonitrile is HPLC level acetonitrile.