CN111366658A - Method for rapidly detecting plasticizer in beef tallow - Google Patents
Method for rapidly detecting plasticizer in beef tallow Download PDFInfo
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- CN111366658A CN111366658A CN202010293458.6A CN202010293458A CN111366658A CN 111366658 A CN111366658 A CN 111366658A CN 202010293458 A CN202010293458 A CN 202010293458A CN 111366658 A CN111366658 A CN 111366658A
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- beef tallow
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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
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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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Abstract
The invention relates to the field of plasticizer detection, in particular to a rapid and accurate plasticizer detection method. Animal fat is used as a detection object, acetonitrile and n-hexane are used as extraction solvents, the plasticizer in the beef tallow is extracted in an ultrasonic-assisted extraction mode, the beef tallow is frozen, and then the plasticizer in the beef tallow is obtained through centrifugation and rapid separation extraction. The method optimizes the sample pretreatment mode in GB 5009.271-2016, can save pretreatment time and SPE silica gel small column cost in the field of plasticizer detection of animal fat, saves consumption of a large amount of reagents, and has accurate detection results.
Description
Technical Field
The invention relates to the field of plasticizer detection, and particularly relates to a scheme for rapidly detecting a plasticizer in beef tallow.
Background
The plasticizer, also called plasticizer, is a polymer material auxiliary agent widely used in industry, and is a chemical agent frequently used in plastic products. Plasticizers are easily dissolved in edible oils, and when plastic packages contain excessive amounts of plasticizers, the edible oils and fats are easily contaminated with plasticizers by migration. The plasticizer is an "environmental hormone", also called "environmental hormone", and trace of such substances remained in the environment enter the human body through the food chain to form a pseudo-hormone, transmit a pseudo-chemical signal, and influence the hormone content in the human body, thereby interfering the original mechanism of human endocrine and causing endocrine dyscrasia.
With the development of the chafing dish industry, more and more people love chafing dishes, particularly beef tallow chafing dishes in Chongqing areas, are deeply loved by people due to the unique beef tallow flavor. The preparation of the hotpot condiment comprises the steps of frying the raw materials such as beef tallow, spice, hot pepper, bean sauce and the like, wherein the beef tallow is the main raw material of the hotpot condiment, and the plastic product is contacted in the production process link from the production and processing of the beef tallow to the frying of the beef tallow hotpot condiment, and is easy to cause migration under the high-temperature condition, so that the plasticizer content in the beef tallow and the hotpot condiment exceeds the related limit standard of China, and the food safety risk is brought to production enterprises. Therefore, the method for rapidly detecting the beef tallow plasticizer can effectively solve the problem that a production enterprise rapidly monitors the risk of the plasticizer in the production process, shortens the pretreatment time, reduces the detection cost, and ensures the beef tallow production enterprise to control the beef tallow quality.
Disclosure of Invention
The invention provides a rapid detection scheme of a beef fat plasticizer, and aims to provide a rapid and accurate plasticizer detection method, which is suitable for fats or fat products with high saturated fatty acid content (more than 50%) or melting points of 41-47 ℃, and animal fat production enterprises can rapidly monitor the plasticizer content and effectively control the plasticizer risk in the production process.
The technical problem to be solved by the invention is realized by adopting the following technical scheme: a method for rapidly detecting a butter plasticizer comprises the following steps: accurately weighing 0.5 g (accurate to 0.001 g) of beef tallow into a 10 mL test tube, preheating and melting the beef tallow in a solidified state before weighing, preheating for 10 min at 50 ℃, and continuously stirring the beef tallow by using a glass rod during weighing to fully and uniformly mix the beef tallow.
Accurately transferring 100 mu L of chromatographically pure hexane and 5 mL of chromatographically pure acetonitrile into a test tube filled with beef tallow, putting the test tube into a 75 ℃ water bath kettle, heating for 1min to melt the beef tallow, and carrying out vortex oscillation for 2 min.
Mixing with beef tallow, and ultrasonic extracting for 15 min.
After the ultrasonic treatment of the sample, immediately putting the sample into a refrigerator with the temperature of 20 ℃ below zero, and freezing for 15-30 min.
Slowly pouring the extraction solvent in the frozen sample into a 10 mL centrifuge tube, and centrifuging for 5 min at 5000 r/min.
After the sample is centrifuged, the upper layer liquid (1-2 mL) is removed by using an injector, and then filtered into a 2mL chromatographic sample bottle by using a 0.22 μm filter head, and the sample is tested at 4 ℃.
Placing a sample to be detected on a sample plate of a gas chromatography-mass spectrometer, setting a column incubator, a sample inlet, a mass spectrum and an ion source temperature, wherein the sample inlet amount is 1 mu L, and the detection time is 26 min. .
According to the invention, the plasticizer extraction time is greatly saved, and the reason that the butter has high saturated fatty acid content and is easy to solidify at normal temperature due to the melting point characteristic of the butter is utilized, the centrifugal separation method is replaced by the SPE small column filtration extraction method in the standard method, so that the sample detection cost and time are greatly saved, and the quality control efficiency of a production enterprise is improved.
Detailed Description
The present invention will now be described with reference to examples.
The scheme for rapidly detecting the plasticizer in the beef tallow comprises the following steps:
preparing reagents and equipment: the device comprises chromatographically pure acetonitrile, chromatographically pure hexane, an ultrasonic cleaner, a refrigerator, a pipette gun, a vortex oscillator, a high-speed centrifuge, a gas chromatography-mass spectrometer, an organic filter head and an injector.
Selecting a sample: the beef tallow is selected as a detection object, the saturated fatty acid content in the beef tallow is high, the melting point is high, the beef tallow is easy to solidify at normal temperature, and the advantages of the beef tallow can be utilized to separate the plasticizer from the extracting solution.
Weighing a sample: accurately weighing 0.5 g (accurate to 0.001 g) of beef tallow into a 10 mL test tube, preheating and melting the beef tallow in a solidified state before weighing, preheating for 10 min at 50 ℃, and continuously stirring the beef tallow by using a glass rod during weighing to fully and uniformly mix the beef tallow.
Adding a reagent: accurately transferring 100 mu L of chromatographically pure hexane and 5 mL of chromatographically pure acetonitrile into a test tube filled with beef tallow, putting the test tube into a 75 ℃ water bath kettle, heating for 1min to melt the beef tallow, and carrying out vortex oscillation for 2 min.
Ultrasonic extraction: mixing with beef tallow, and ultrasonic extracting for 15 min.
Freezing treatment: and (3) after the sample is subjected to ultrasonic treatment, immediately putting the sample into a refrigerator with the temperature of-20 ℃, and freezing for 15-30 min.
Freezing and centrifuging: slowly pouring the extraction solvent in the frozen sample into a 10 mL centrifuge tube, and centrifuging for 5 min at 5000 r/min.
And (3) filtering treatment: after the sample is centrifuged, the upper layer liquid (1-2 mL) is removed by using an injector, and then filtered into a 2mL chromatographic sample bottle by using a 0.22 μm filter head, and the sample is tested at 4 ℃.
Sample introduction detection: placing a sample to be detected on a sample plate of a gas chromatography-mass spectrometer, setting a column incubator, a sample inlet, a mass spectrum and an ion source temperature, wherein the sample inlet amount is 1 mu L, and the detection time is 26 min.
Finally, it should be noted that: the above embodiments are only used to illustrate the present invention and do not limit the technical solutions described in the present invention; thus, while the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted; all such modifications and variations are intended to be included herein within the scope of this disclosure and the present invention and protected by the following claims.
Claims (10)
1. A method for rapidly detecting a plasticizer in beef tallow is characterized in that the reagents and equipment comprise the following components: the device comprises chromatographically pure acetonitrile, chromatographically pure hexane, an ultrasonic cleaner, a refrigerator, a pipette gun, a vortex oscillator, a high-speed centrifuge, a gas chromatography-mass spectrometer, an organic filter head and an injector.
2. The plasticizer detection method according to claim 1, wherein: the animal fat is selected as a detection object, the saturated fatty acid content of the animal fat is high, the animal fat is solid at normal temperature, the melting point is 41-47 ℃, and the plasticizer can be quickly separated and extracted by utilizing the physical advantages of the animal fat.
3. The method for rapidly detecting the plasticizer in the beef tallow according to claim 1, wherein the method comprises the following steps: accurately weighing 0.5 g (accurate to 0.001 g) of beef tallow into a 10 mL test tube, preheating and melting the beef tallow in a solidified state before weighing, wherein the temperature is about 50 ℃, the preheating is about 5 min, continuously stirring the beef tallow by using a glass rod during weighing to fully mix the beef tallow, and sampling for a small amount of times.
4. The method for rapidly detecting the plasticizer in the beef tallow according to claim 1, wherein the method comprises the following steps: accurately transferring 100 mu L of chromatographically pure hexane and 5 mL of chromatographically pure acetonitrile into a test tube with weighed beef tallow, putting the test tube into a 75 ℃ water bath kettle, heating for 1min to melt the beef tallow, and carrying out vortex oscillation for 2 min to fully and uniformly mix the grease and the solvent.
5. The method for detecting beef tallow plasticizer according to claim 1, wherein the method comprises the following steps: mixing with beef tallow, and ultrasonic extracting for 15 min.
6. The method for rapidly detecting the plasticizer in the beef tallow according to claim 1, wherein the method comprises the following steps: and (3) after the sample is subjected to ultrasonic treatment, immediately putting the sample into a refrigerator with the temperature of-20 ℃, and freezing for 15-30 min.
7. The method for rapidly detecting the plasticizer in the beef tallow according to claim 1, wherein the method comprises the following steps: slowly pouring the extraction solvent in the frozen sample into a 10 mL centrifuge tube, and centrifuging for 5 min at 5000 r/min.
8. The method for rapidly detecting the plasticizer in the beef tallow according to claim 1, wherein the method comprises the following steps: after the sample is centrifuged, the upper layer liquid (1-2 mL) is removed by using an injector, and then filtered into a 2mL chromatographic sample bottle by using a 0.22 μm filter head, and the sample is tested at 4 ℃.
9. The method for rapidly detecting the plasticizer in the beef tallow according to claim 1, wherein the method comprises the following steps: placing a sample to be detected on a sample plate of a gas chromatography-mass spectrometer, setting a column incubator, a sample inlet, a mass spectrum and an ion source temperature, wherein the sample inlet amount is 1 mu L, and the detection time is 26 min.
10. The method for rapidly detecting the plasticizer in the beef tallow according to claim 1, wherein the method comprises the following steps: compared with the national standard method, the method uses 5.1 mL of reagent, the sample treatment and detection time is about 70 min, the consumed reagent and time are greatly saved, a centrifugal separation mode is used, an SPE solid phase extraction mode in the standard method is replaced, the detection cost is saved, the final detection result is accurate, the detection limit and the quantitative limit are good, and the recovery rate is good.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010293458.6A CN111366658A (en) | 2020-04-15 | 2020-04-15 | Method for rapidly detecting plasticizer in beef tallow |
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| CN202010293458.6A CN111366658A (en) | 2020-04-15 | 2020-04-15 | Method for rapidly detecting plasticizer in beef tallow |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102620978A (en) * | 2012-04-09 | 2012-08-01 | 天津春发生物科技集团有限公司 | Matrix dispersion solid phase extraction method for detection of plasticizer in animal and vegetable oil samples |
| CN103335878A (en) * | 2013-05-06 | 2013-10-02 | 江南大学 | Pre-treatment method for phthalate ester plasticizers in edible oil |
| CN105911172A (en) * | 2016-04-14 | 2016-08-31 | 北京工商大学 | Method for rapid detection of plasticizer in sorghum |
| CN107917977A (en) * | 2017-12-12 | 2018-04-17 | 山东金胜粮油集团有限公司 | A kind of method for quickly detecting of grease plasticiser |
-
2020
- 2020-04-15 CN CN202010293458.6A patent/CN111366658A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102620978A (en) * | 2012-04-09 | 2012-08-01 | 天津春发生物科技集团有限公司 | Matrix dispersion solid phase extraction method for detection of plasticizer in animal and vegetable oil samples |
| CN103335878A (en) * | 2013-05-06 | 2013-10-02 | 江南大学 | Pre-treatment method for phthalate ester plasticizers in edible oil |
| CN105911172A (en) * | 2016-04-14 | 2016-08-31 | 北京工商大学 | Method for rapid detection of plasticizer in sorghum |
| CN107917977A (en) * | 2017-12-12 | 2018-04-17 | 山东金胜粮油集团有限公司 | A kind of method for quickly detecting of grease plasticiser |
Non-Patent Citations (3)
| Title |
|---|
| 中华人民共和国国家卫生和计划生育委员会等: "食品安全国家标准 食品中邻苯二甲酸酯的测定", 《GB5009.271-2016》 * |
| 李旭等: "气相色谱串联质谱法测定植物油中的邻苯二甲酸酯", 《食品工业》 * |
| 赵云霞等: "GC-MS 同时测定油脂性的食品及食品添加剂中16种邻苯二甲酸酯类迁移物", 《分析试验室》 * |
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