CN108845052A - Determination of Preservatives detection method of content in a kind of solid food - Google Patents
Determination of Preservatives detection method of content in a kind of solid food Download PDFInfo
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- CN108845052A CN108845052A CN201810726687.5A CN201810726687A CN108845052A CN 108845052 A CN108845052 A CN 108845052A CN 201810726687 A CN201810726687 A CN 201810726687A CN 108845052 A CN108845052 A CN 108845052A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention belongs to technical field of food detection, and in particular to Determination of Preservatives detection method of content in a kind of solid food.The present invention sample to be tested is smashed to pieces after with saturated sodium-chloride water solution make protein formed precipitating remove, fat constituent is removed by n-hexane extraction again, adsorbent is taken to be parsed with ethyl alcohol after adsorbent concussion centrifugation is added, acetone constant volume is used after drying, is detected after filter membrane with the gas chromatograph equipped with hydrogen flame detector.The present invention can effectively remove the interference component in sample to be tested in such a way that protein precipitation, n-hexane extraction fat constituent and adsorbent further purify, and can detect 12 kinds of preservatives in sample to be tested simultaneously.
Description
Technical field
The invention belongs to preservative detection technique fields, and in particular to Determination of Preservatives content detection in a kind of solid food
Method.
Background technique
Preservative (preservative) refers to the medicament of inhibiting substances corruption, i.e., to using corrupt substance as metabolism substrate
The growth of microorganism has lasting inhibiting effect, is widely used in the fields such as food, daily use chemicals.It is allowed to addition in the world
There are many preservative type, and if the U.S. is there are about 50 kinds, Japan has 40 kinds.At present China only have approved 32 kinds allow using food it is anti-
Rotten agent, they are going through all to have passed through a large amount of scientific experiment using preceding, are less toxic, the higher kind of safety, mainly
Including：Benzoic acid and sodium benzoate, sorbic acid and its sylvite, sulfur dioxide, sodium pyrosulfite (potassium), sodium propionate (calcium), to hydroxyl
Benzoates, dehydroacetic acid etc.；What wherein application was more is sorbic acid and benzoic acid and its esters.In addition, there are also some days
Right biological preservative such as nisin, natamycin, chitosan etc. and novel preservative, such as dimethyl fumarate
Deng.As long as food preservative used in food production manufacturer is strict controlled in national standard in terms of kind, quantity and range
《Food additives use sanitary standard》(GB2760-2011) within the scope of as defined in, it should will not cause to damage to human health
Evil, product can trust edible.But it is regrettable and extremely worry, numerous food product manufacturing enterprise is due to being produced into
The not high influence of this limitation and practitioner's quality, and to the no concept of the harm of preservative in consciousness, therefore exist
In violation of rules and regulations, illegal abuse, abuse, the phenomenon that overdose is using food preservative, cause many food to become additive and wherein also wrap
" the integrated hodgepodge " of preservative is included, excessively intake can bring certain negative effect to health；Indiscriminate adding preservative agent can be right
Society and consumer generate great influence.Therefore a set of detection technique standard quickly, accurate, easy, inexpensive is established, with
It is widely used in several based foods such as beverage, cake, flavouring, preserved fruit, the detection efficiency of preservative in food can be improved, and can have
The control testing cost of effect shortens detection cycle, is conducive to the reasonable employment of preservative and market circulation in enterprise production process
Fast slowdown monitoring of the law enforcement agency to preservative addition situation in the process；Ensuring that food security aspect has great importance,
Social benefit is very significant.Due to different preservatives, its structural property is also not quite similar, and the sample substrate being additionally present of is also complicated
Therefore, in current standard multiplicity is directed to different preservatives and using the detection means in different food types also each not phase
Together.The detection preservative standard of present is many kinds of, and the experiment condition being related to is also different, and the preservative type being directed to
Also relatively simple, it tends not to once quickly detect a variety of Determination of common preservatives, causes round of visits to lengthen, reduce the effect of investigation
Rate.The method of usually detection preservative has liquid chromatography, Liquid Chromatography-Mass Spectrometry, gas chromatography and gas-chromatography-
Mass Spectrometry etc..Although liquid chromatography, Liquid Chromatography-Mass Spectrometry can measure Determination of Preservatives simultaneously, due to
Food samples matrix species are various, and matrix will lead to interference, be easy to cause false positive or false negative result, and it is accurate to influence
It is quantitative.Gas chromatography-mass spectrometry is higher to instrument requirements, should not promote the use of.
Summary of the invention
The object of the present invention is to provide Determination of Preservatives detection method of content in a kind of solid food.Sample to be tested is smashed to pieces
Make protein form precipitating with saturated sodium-chloride water solution afterwards to remove, then fat constituent is removed by n-hexane extraction, is added and inhales
It takes adsorbent to be parsed with ethyl alcohol after attached dose of concussion centrifugation, acetone constant volume is used after drying, is used after filter membrane and is furnished with hydrogen flame detector
Gas chromatograph detection.
The technical scheme is that：
Determination of Preservatives detection method of content in a kind of solid food, includes the following steps：
(1) it takes sample to be tested to smash into powder to pieces, sample to be tested is added in saturated sodium chloride solution and is placed in ultrasonic wave
It is shaken in concussion instrument, it is 4~5 that dust technology, which is added, and adjusts pH, so that protein is formed precipitating, is filtered to remove insoluble matter；
(2) n-hexane is added in filtrate and carries out time extraction, isolates fat；
(3) adsorbent is added into extraction raffinate, concussion, centrifugation take adsorbent, are obtained with EtOH Sonicate concussion parsing
Desorbed solution；
(4) desorbed solution with after being dried with nitrogen with acetone constant volume, with the gas-chromatography equipped with hydrogen flame detector after filter membrane
Instrument detection.
Preferably, the ultrasonic vibration time is 2~5min in step (1).
Preferably, adsorbent and the w/v of filtrate are in step (3)：0.2g/L~0.8g/L.
Preferably, the adsorbent is the mixture of carbon nano-fiber, alkylamino silica gel and graphene oxide.
It is highly preferred that the weight ratio of carbon nano-fiber in the adsorbent, alkylamino silica gel, graphene oxide is：1~2:2
~3:5~8.
Preferably, the w/v of adsorbent and ethyl alcohol is in step (3)：2g/L~5g/L.
Preferably, the concussion time is 30~50min in step (3).
Preferably, filter membrane refers to that aperture is the filter membrane of 0.45um in step (4).
Preferably, the preservative include propionic acid, it is sorbic acid, benzoic acid, dehydroactic acid, methyl p-hydroxybenzoate, right
Nipagin A, propylparaben, p-Hydroxybenzoic acid isopropyl ester, butyl p-hydroxybenzoate, para hydroxybenzene
Iso-butyl formate, n Heptyl p hydroxybenzoate and dimethyl fumarate.
Beneficial effects of the present invention are as follows：
The present invention, can in such a way that protein precipitation, n-hexane extraction fat constituent and adsorbent further purify
The interference component in sample to be tested is effectively removed, 12 kinds of preservatives in sample to be tested can be detected simultaneously.
Specific embodiment
With reference to embodiment, technical solution of the present invention is described in further detail, but do not constituted pair
Any restrictions of the invention.
Embodiment 1
Determination of Preservatives detection method of content in a kind of solid food, includes the following steps：
(1) 5.00g sample to be tested is taken to smash into powder to pieces, sample to be tested is added in saturated sodium chloride solution be placed in it is super
5min is shaken in sound wave shock instrument, it is 4~5 that dust technology, which is added, and adjusts pH, so that protein is formed precipitating, is filtered to remove insoluble matter；
(2) n-hexane is added in filtrate and carries out time extraction, isolates fat；
(3) adsorbent is added into extraction raffinate, adsorbent is that weight ratio is 1:2:6 carbon nano-fiber, amino silicone
The ratio of the mixture of glue and graphene oxide, adsorbent additional amount and extraction raffinate is 0.3g/L, shakes 40min, then
Centrifugation, takes adsorbent, is parsed with EtOH Sonicate concussion and obtains desorbed solution, and the ratio of adsorbent and amount of alcohol added is 2g/L；
(4) desorbed solution is settled to 5mL with acetone with after being dried with nitrogen, cross after the filter membrane that aperture is 0.45um obtain it is to be measured
Liquid.
(5) chromatographic parameter is set as：
Chromatographic column：0.25 μm of the μ m of HP-innowax, 30m × 320；
Column temperature：130 DEG C of initial temperature, 170 DEG C are risen to 10 DEG C/min, 3min is stopped, then rise to 260 DEG C with 20 DEG C/min, stops
Stay 21.5min；
Injector temperature：250℃；
Detector：FID
Detector temperature：260℃；
Carrier gas：High-purity N 2, flow velocity 0.8mL/min；
Sample volume：1μL；Split ratio：10:1.
(6) weigh respectively preservative propionic acid, sorbic acid, benzoic acid, dehydroactic acid, methyl p-hydroxybenzoate, to hydroxyl
Ethyl benzoate, propylparaben, p-Hydroxybenzoic acid isopropyl ester, butyl p-hydroxybenzoate, P-hydroxybenzoic acid
Isobutyl ester, n Heptyl p hydroxybenzoate and dimethyl fumarate standard items 0.2000g, with acetone solution and are diluted to 100mL, make
Each preservative Standard Stock solutions concentration is respectively 2mg/mL；Pipette respectively preservative standard reserving solution 0.1mL, 0.2mL,
0.5mL, 1.0mL, 2.0mL, 5.0mL are settled to 5.0mL in 6 5.0mL volumetric flasks, with acetone, prepare hybrid standard work
Liquid series, making the ultimate density of each preservative is respectively 0.04mg/mL, 0.08mg/mL, 0.2mg/mL, 0.4mg/mL, 1.0mg/
mL,2.5mg/mL；
(7) above-mentioned hybrid standard working solution is pressed into concentration sample detection from low to high, with peak area-concentration mapping, obtained
To standard curve regression equation, using the concentration of each preservative as abscissa, using corresponding peak area as ordinate, linearly returned
Return, linear concentration range is 0.04-2.50mg/mL.According to 3 times of signal-to-noise ratio, actually to weigh sample 5.00g, finally it is settled to
5.0mL, the equation of linear regression coefficient R of various preservatives2Within the scope of 0.99890-0.99960, minimum detectability
0.85-4.81mg/kg, detection limit meet the daily detection requirement of preservative in food.
(8) it is operated by the method for the present invention, add hybrid standard working solution in the sample and carries out 6 parallel determinations respectively,
The measurement repeatability for measuring antiseptic content in sample is good, and RSD value is respectively less than 5.0%, and the rate of recovery is also in 92.6%-
Between 98.5%.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (9)
1. Determination of Preservatives detection method of content in a kind of solid food, which is characterized in that include the following steps：
(1) it takes sample to be tested to smash into powder to pieces, sample to be tested is added in saturated sodium chloride solution and is placed in ultrasonic oscillation
It is shaken in instrument, it is 4~5 that dust technology, which is added, and adjusts pH, so that protein is formed precipitating, is filtered to remove insoluble matter；
(2) n-hexane is added in filtrate and carries out time extraction, isolates fat；
(3) adsorbent is added into extraction raffinate, concussion, centrifugation take adsorbent, are parsed with EtOH Sonicate concussion
Liquid；
(4) desorbed solution after filter membrane with the gas chromatograph equipped with hydrogen flame detector with acetone constant volume, being examined after being dried with nitrogen
It surveys.
2. Determination of Preservatives detection method of content in a kind of solid food according to claim 1, which is characterized in that step
(1) the ultrasonic vibration time is 2~5min in.
3. Determination of Preservatives detection method of content in a kind of solid food according to claim 1, which is characterized in that step
(3) adsorbent and the w/v of filtrate are in：0.2g/L~0.8g/L.
4. Determination of Preservatives detection method of content in a kind of solid food according to claim 1, which is characterized in that described
Adsorbent is the mixture of carbon nano-fiber, alkylamino silica gel and graphene oxide.
5. Determination of Preservatives detection method of content in a kind of solid food according to claim 4, which is characterized in that described
Carbon nano-fiber in adsorbent, alkylamino silica gel, graphene oxide weight ratio be：1~2:2~3:5~8.
6. Determination of Preservatives detection method of content in a kind of solid food according to claim 1, which is characterized in that step
(3) w/v of adsorbent and ethyl alcohol is in：2g/L~5g/L.
7. Determination of Preservatives detection method of content in a kind of solid food according to claim 1, which is characterized in that step
(3) the concussion time is 30~50min in.
8. Determination of Preservatives detection method of content in a kind of solid food according to claim 1, which is characterized in that step
(4) filter membrane refers to that aperture is the filter membrane of 0.45um in.
9. Determination of Preservatives detection method of content in a kind of solid food according to claim 1, which is characterized in that described
Preservative include propionic acid, sorbic acid, benzoic acid, dehydroactic acid, methyl p-hydroxybenzoate, ethyl-para-hydroxybenzoate, to hydroxyl
Yl benzoic acid propyl ester, p-Hydroxybenzoic acid isopropyl ester, butyl p-hydroxybenzoate, p-Hydroxybenzoic acid isobutyl ester, para hydroxybenzene
Heptyl formate and dimethyl fumarate.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112649528A (en) * | 2020-12-14 | 2021-04-13 | 安徽中青检验检测有限公司 | Food preservative content safety detection method |
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| EP0319454A2 (en) * | 1987-11-30 | 1989-06-07 | Sekisui Kagaku Kogyo Kabushiki Kaisha | An eliminating agent for glycosylated hemoglobin |
| CN101532995A (en) * | 2009-05-04 | 2009-09-16 | 佛山市海天调味食品有限公司 | Method for determining antiseptic content rapidly in spice with grease |
| CN103076407A (en) * | 2012-12-26 | 2013-05-01 | 通标标准技术服务有限公司 | Fast detection method for food preservative agent and antioxidant |
| CN107202724A (en) * | 2017-07-11 | 2017-09-26 | 安徽宏远职业卫生技术服务有限公司 | The sample pretreating method of preservative in a kind of detection fruit juice |
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2018
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0319454A2 (en) * | 1987-11-30 | 1989-06-07 | Sekisui Kagaku Kogyo Kabushiki Kaisha | An eliminating agent for glycosylated hemoglobin |
| CN101532995A (en) * | 2009-05-04 | 2009-09-16 | 佛山市海天调味食品有限公司 | Method for determining antiseptic content rapidly in spice with grease |
| CN103076407A (en) * | 2012-12-26 | 2013-05-01 | 通标标准技术服务有限公司 | Fast detection method for food preservative agent and antioxidant |
| CN107202724A (en) * | 2017-07-11 | 2017-09-26 | 安徽宏远职业卫生技术服务有限公司 | The sample pretreating method of preservative in a kind of detection fruit juice |
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|---|
| 孙颖霞 等: "气相色谱法测定果蔬饮料中6中防腐剂", 《中国测试》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112649528A (en) * | 2020-12-14 | 2021-04-13 | 安徽中青检验检测有限公司 | Food preservative content safety detection method |
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Application publication date: 20181120 |