CN209858497U - Pretreatment and analysis integrated device for online detection of benzo (a) pyrene in hot-pressed vegetable oil - Google Patents
Pretreatment and analysis integrated device for online detection of benzo (a) pyrene in hot-pressed vegetable oil Download PDFInfo
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- CN209858497U CN209858497U CN201920566185.0U CN201920566185U CN209858497U CN 209858497 U CN209858497 U CN 209858497U CN 201920566185 U CN201920566185 U CN 201920566185U CN 209858497 U CN209858497 U CN 209858497U
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Abstract
The utility model discloses an integrative device of pretreatment and analysis of benzo (a) pyrene in on-line measuring hot pressed vegetable oil, including the automatic sample injector, two chromatographic pumps, six-way valve, on-line purification post, the chromatogram separation post, fluorescence detector, six interfaces that are used for the six-way valve that the system switches are a respectively in proper order, b, c, d, e, f, the automatic sample injector links to each other with first chromatographic pump and six-way valve interface an respectively, even have the second chromatographic pump on the six-way valve interface d, the second chromatographic pump and first stock solution bottle, the second stock solution bottle links to each other, it has chromatogram separation post and fluorescence detector to link to each other in proper order on the six-way valve interface c, be connected with on-line purification post between six-way valve interface b and the interface e, six-way valve interface f is the waste liquid interface, be connected with the third stock solution bottle on the first chromatographic pump respectively, fourth stock solution bottle and fifth stock solution. Can be directly detected without pretreatment, thereby greatly reducing the analysis cost.
Description
Technical Field
The utility model relates to an online analysis device especially relates to a with hot-pressed vegetable oil direct injection device, purifies on line and sample analysis and need not carry out the pretreatment and the integrative device of analysis of benzo (a) pyrene in the on-line measuring hot-pressed vegetable oil of pretreatment to the sample.
Background
Benzo (a) pyrene (BaP) is the first discovered environmental chemical carcinogen, has strong carcinogenicity, is one of three generally recognized carcinogens in the world, can cause various cancers such as lung cancer, gastric cancer, bladder cancer, digestive tract cancer and the like, has teratogenicity and mutagenicity, and can influence offspring through a mother body via placenta so as to cause embryo malformation or death and immunologic function reduction. Vegetable oil is an indispensable cooking material in daily diet of people, and the food safety problem is not easy to be overlooked. The source of BaP in vegetable oils is a variety of factors, such as environmental factors, processing and packaging transportation factors. In which hot-pressed vegetable oil seeds are required to be roasted, roasted or steamed in the drying stage, BaP may be formed if the temperature is not properly controlled, and the leaching method may also be carried out with the organic solvent itself containing BaP into the vegetable oil. GB 2762 and 2017 pollutant limit in national food safety standards stipulate that the BaP limit in the grease and products thereof is 10 mu g/kg. European Union regulation No 835/2011 stipulates that the content of BaP in other fats and oils is less than or equal to 2 μ g/kg in addition to cacao butter and coconut oil, and BaP in perilla oil and sesame oil is less than 2.0 μ g/kg in Korea, so that there is an event that perilla oil and sesame oil exported to Korea is recalled because BaP exceeds the standard.
The detection methods of BaP are various, and mainly include thin layer chromatography, fluorescence spectrophotometry, high performance liquid chromatography, gas chromatography-mass spectrometry and the like. After many revisions, the existing national standard GB 5009.27-2016 (determination of benzo (a) pyrene in food safety national standard food) abandons part of older detection methods, and a liquid chromatography-fluorescence detector method is adopted for determination. According to the standard, the oil and the products thereof are dissolved by normal hexane, and are enriched and purified by a neutral alumina column or a molecular imprinting column, so that the operation is complicated and time-consuming, the solvent toxicity is high, particularly the activity of the neutral alumina column is difficult to control, and the recovery rate is unstable. And if a large amount of organic solvent is used, if the reagent is not pure with BaP residue, the reagent is concentrated and enriched after elution, and false positive condition is easy to occur. Therefore, the existing method for monitoring benzo (a) pyrene in hot-pressed vegetable oil generally has the problems of complicated operation, unstable recovery rate, easy occurrence of false positive due to impure reagent, high cost of pretreatment column and the like.
If the pretreatment direct analysis of the hot-pressed vegetable oil is not needed, the pretreatment and the analysis are carried out on line through the on-line detection equipment, the error of manual operation can be effectively reduced, the pretreatment time is shortened, the detection efficiency is improved, the detection accuracy is improved, and the use cost is reduced.
SUMMERY OF THE UTILITY MODEL
The utility model aims to solve the technical problem that a pretreatment and the integrative device of analysis of benzo (a) pyrene in on-line measuring hot-pressing vegetable oil are provided, will hot-pressing vegetable oil direct injection device, purify and the sample analysis on line, need not carry out the pretreatment to the sample, make benzo (a) pyrene analysis easy and simple to handle in the hot-pressing vegetable oil, improve detection efficiency, the material resources of using manpower sparingly reduce use cost.
In order to solve the technical problem, the utility model discloses a technical scheme is: the utility model provides an integrative device of preliminary treatment and analysis of benzo (a) pyrene in on-line measuring hot-pressed vegetable oil, including automatic sample injector, two chromatographic pumps, six-way valve, on-line purification post, chromatographic separation post, fluorescence detector, six interfaces of six-way valve for system's switching are a in proper order respectively, b, c, d, e, f, automatic sample injector links to each other with first chromatographic pump and six-way valve interface a respectively, even have the second chromatographic pump on six-way valve interface d, the second chromatographic pump links to each other with first stock solution bottle, second stock solution bottle, even have chromatographic separation post and fluorescence detector on six-way valve interface c in proper order, be connected with on-line purification post between six-way valve interface b and the interface e, six-way valve interface f is the waste liquid interface, be connected with third stock solution bottle, fourth stock solution bottle and fifth stock solution bottle on the first chromatographic pump respectively.
First stock solution bottle is used for adorning the acetonitrile, and the second stock solution bottle is used for adorning water, and the third stock solution bottle is used for adorning the acetonitrile, and the fourth stock solution bottle is used for adorning water, and the fifth stock solution bottle is used for adorning isopropanol.
The first chromatographic pump is a ternary gradient pump or a quaternary gradient pump and is used for respectively conveying acetonitrile in a third liquid storage bottle, water in a fourth liquid storage bottle and isopropanol in a fifth liquid storage bottle; the second chromatographic pump is a quaternary gradient pump and is used for respectively conveying acetonitrile in the first liquid storage bottle and water in the second liquid storage bottle.
The detection method of the pretreatment and analysis integrated device for online detection of benzo (a) pyrene in hot-pressed vegetable oil sequentially comprises the following steps:
(1) sample introduction and system balance process: the automatic sample injector enables a sample injection system to enter a six-way valve along with isopropanol in a fifth liquid storage bottle in the first chromatographic pump, benzo (a) pyrene in the sample is enriched in an online purification column, and impurities and matrixes are discharged into waste liquid along with the isopropanol; the second chromatographic pump brings mobile phases in the first bottle liquid and the second bottle liquid into the six-way valve, the chromatographic separation column and the fluorescence detector, and the whole system is balanced;
(2) elution analysis process: the six-way valve switches, and the second chromatogram pump gets into the mobile phase in the first stock solution bottle and the second stock solution bottle and links to on-line purifying column on the six-way valve, and benzo (a) pyrene in the on-line purifying column gets into the chromatogram separation column and separates to carry out the analysis through fluorescence detector.
The utility model has the advantages that: the hot-pressed vegetable oil can be directly injected into the device for on-line purification and sample analysis without pretreatment of the sample. The problems that the time consumption is long, the reagent consumption is large, the material consumption cost is high, the experiment condition is not easy to control and the like in the traditional method for detecting benzo (a) pyrene by adopting a liquid chromatography are solved. The analysis method has the advantages of simple and convenient analysis operation of benzo (a) pyrene in hot-pressed vegetable oil, improvement of detection efficiency, manpower and material resource saving and reduction of use cost. Meanwhile, the online purification pretreatment device saves the time and the complicated operation process of sample pretreatment, and the online purification column is activated, regenerated and recycled, so that the online purification column is more environment-friendly compared with the disposable use characteristic of the traditional purification column, and the analysis cost is greatly reduced.
Drawings
FIG. 1 is a schematic diagram of the sample introduction and system balance process of the on-line detection and analysis integrated device for benzo (a) pyrene in hot-pressed vegetable oil.
FIG. 2 is the structure diagram of the elution analysis process of the pretreatment and analysis integrated device for on-line detection of benzo (a) pyrene in hot-pressed vegetable oil.
FIG. 3 is a chromatogram for analyzing benzo (a) pyrene in hot-pressed vegetable oil according to an embodiment of the present invention.
Fig. 4 is a calibration graph of benzo (a) pyrene according to an embodiment of the present invention.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to the accompanying drawings and the detailed description below:
as shown in figures 1 and 2, the utility model discloses an integrative device of pretreatment and analysis of benzo (a) pyrene in on-line measuring hot pressed vegetable oil, including automatic sample injector, two chromatographic pumps, six way valve, on-line purification post, chromatographic fractionation post, fluorescence detector, six interfaces of six way valve 3 for system's switching are a, b, c, d, e, f respectively in proper order, automatic sample injector 2 links to each other with first chromatographic pump 1 and six way valve 3 interface a respectively, even have second chromatographic pump 4 on six way valve 3 interface d, second chromatographic pump 4 links to each other with first stock solution bottle 11, second stock solution bottle 12, even have chromatographic fractionation post 5 and fluorescence detector 6 in proper order on six way valve 3 interface c, be connected with on-line purification post 7 between six way valve 3 interface b and the interface e, six way valve 3 interface f is the waste liquid interface, be connected with third stock solution bottle 8 respectively on the first chromatographic pump 1, A fourth liquid storage bottle 9 and a fifth liquid storage bottle 10.
First stock solution bottle 11 is used for adorning the acetonitrile, and second stock solution bottle 12 is used for adorning the water, and third stock solution bottle 8 is used for adorning the acetonitrile, and fourth stock solution bottle 9 is used for adorning the water, and fifth stock solution bottle 10 is used for adorning isopropanol.
The first chromatographic pump 1 is a ternary gradient pump or a quaternary gradient pump and is used for respectively conveying acetonitrile in a third liquid storage bottle 8, water in a fourth liquid storage bottle 9 and isopropanol in a fifth liquid storage bottle 10; the second chromatographic pump 4 is a quaternary gradient pump and is used for respectively conveying acetonitrile in the first liquid storage bottle 11 and water in the second liquid storage bottle 12.
The detection method of the pretreatment and analysis integrated device for online detection of benzo (a) pyrene in hot-pressed vegetable oil sequentially comprises the following steps:
(1) sample introduction and system balance process: the automatic sample injector 2 enables a sample injection system to enter the six-way valve 3 along with isopropanol in the fifth liquid storage bottle 10 in the first chromatographic pump 1, benzo (a) pyrene in the sample is enriched in the online purification column 7, and impurities and matrixes are discharged into waste liquid along with the isopropanol; the second chromatographic pump 4 brings mobile phases in the first bottle liquid 11 and the second bottle liquid 12 into the six-way valve 3, the chromatographic separation column 5 and the fluorescence detector 6, and the whole system is balanced;
(2) elution analysis process: the six-way valve 3 switches, and the second chromatographic pump 4 gets into the mobile phase in first stock solution bottle 11 and the second stock solution bottle 12 and links to the online clean column 7 on the six-way valve 3, and the benzo (a) pyrene in the online clean column 7 gets into the separation of chromatogram post 5 and separates to carry out the analysis through fluorescence detector 6.
Examples
(1) Sample introduction and system balance process: injecting 80 mu L of hot-pressed vegetable oil sample into the system by the autosampler 2, feeding the hot-pressed vegetable oil sample into the six-way valve 3 along with isopropanol in a fifth bottle stock solution 10 in the first chromatographic pump 1 at the speed of 0.5mL/min, enriching benzo (a) pyrene in the sample in an online purifying column 7 (model: ChromSpher Pi 3.0mm multiplied by 80mm), and discharging impurities and matrix into waste liquid along with the isopropanol; the second chromatography pump 4 brought the mobile phase (acetonitrile + water 88+12) in the first and second vials 11 and 12 into the six-way valve 3, the chromatography separation column 5 (model: Ultimate PAH4.6mm × 250mm, 5 μm), and the fluorescence detector 6 at a rate of 1.5mL/min, and the whole system was equilibrated.
(2) Elution analysis process: the six-way valve 3 is switched, the second chromatographic pump 4 brings acetonitrile in the first bottle stock 11 and water in the second bottle stock 12 (acetonitrile + water: 88+12) into an online purification column 7 (model: chromasphere Pi 3.0mm × 80mm) on the six-way valve 3 at a rate of 1.5mL/min, the benzo (a) pyrene in the online purification column 7 is eluted into a chromatographic separation column 5 (model: umate PAH4.6mm × 250mm, 5 μm, column temperature: 30 ℃) for separation, and analyzed by a fluorescence detector 6 (excitation wavelength 384nm, emission wavelength 406 nm).
(3) And (3) washing and activating processes of the online purification column: the first chromatographic pump 1 brings acetonitrile in the third bottle reservoir 8 and water in the fourth bottle reservoir 9 into an online purifying column 7 (model: ChromSpher Pi 3.0mm x 80mm) through a six-way valve 3 at a speed of 0.5mL/min (the gradient ratio is shown in the following table), and then the acetonitrile in the third bottle reservoir 8 is switched to wash the online purifying column, and the isopropanol in the fifth bottle reservoir 10 is switched to activate and regenerate the online purifying column for purifying analysis of the next sample. Meanwhile, the second chromatographic pump 4 brings acetonitrile in the first bottle stock 11 and water in the second bottle stock 12 (acetonitrile + water: 88+12) into the six-way valve 3, the chromatographic separation column 5 (model: Ultimate pah4.6mm × 250mm, 5 μm) and the fluorescence detector 6 at a speed of 1.5mL/min, and the chromatographic separation column 5 is balanced.
(4) The cleaning process of the system comprises the following steps: the first chromatographic pump 1 brings acetonitrile in the third bottle stock 8 into an online purifying column 7 (model: ChromSpher Pi 3.0mm × 80mm) through a six-way valve 3 at a speed of 0.5mL/min for cleaning and discharging waste liquid, meanwhile, the second chromatographic pump 4 brings acetonitrile in the first bottle stock 11 into the six-way valve 3, the chromatographic separation column 5 and the fluorescence detector 6 at a speed of 1.0mL/min, the chromatographic separation column 5 (model: Ultimate PAH4.6mm × 250mm, 5 μm) and the fluorescence detector 6 are cleaned, and after cleaning is completed, the flow rates of the first chromatographic pump 1 and the second chromatographic pump 4 are reduced to 0.0mL/min, and sample analysis is finished.
(5) The first chromatography pump 1 reservoir 8, 9, 10 time gradient program is shown in the following table:
(6) the time gradient program of the liquid storage bottle 8 of the chromatographic pump 1 and the liquid storage bottle 11 of the chromatographic pump 4 in the cleaning process of the system is shown in the following table:
| time min | Liquid storage bottle 8 (%) | Liquid storage bottle 11 (%) |
| 0 | 100 | 100 |
| 30 | 100 | 100 |
(7) Drawing a standard curve: calibration curve solutions of 0.5ng/mL, 1.0ng/mL, 5.0ng/mL, 10.0ng/mL, and 20.0ng/mL were prepared with acetonitrile, and linear regression was performed using the mass concentration (X) and the peak area (Y). The linear equation for the calibration curve is 9891.0740X +9.8348, and the linear correlation coefficient R2 is 0.9999. The chromatogram of benzo (a) pyrene is shown in FIG. 3, and the standard curve of benzo (a) pyrene is shown in FIG. 4.
The above-mentioned embodiments are only used for illustrating the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and to implement the present invention accordingly, the scope of the present invention should not be limited by the embodiment, that is, all equivalent changes or modifications made by the spirit of the present invention should still fall within the scope of the present invention.
Claims (3)
1. A pretreatment and analysis integrated device for on-line detection of benzo (a) pyrene in hot-pressed vegetable oil comprises an automatic sample injector, two chromatographic pumps, a six-way valve, an on-line purification column, a chromatographic separation column and a fluorescence detector, and is characterized in that six interfaces of the six-way valve (3) used for system switching are a, b, c, d, e and f in sequence, the automatic sample injector (2) is connected with a first chromatographic pump (1) and an interface a of the six-way valve (3) respectively, a second chromatographic pump (4) is connected with an interface d of the six-way valve (3), the second chromatographic pump (4) is connected with a first liquid storage bottle (11) and a second liquid storage bottle (12), the interface c of the six-way valve (3) is connected with a chromatographic separation column (5) and a fluorescence detector (6) in sequence, the on-line purification column (7) is connected between the interface b and the interface e of the six-way valve (3), and the interface f of the six-way valve (, the first chromatographic pump (1) is respectively connected with a third liquid storage bottle (8), a fourth liquid storage bottle (9) and a fifth liquid storage bottle (10).
2. The integrated device for the on-line detection and analysis of benzo (a) pyrene in hot-pressed vegetable oil according to claim 1, wherein said first liquid storage bottle (11) is used for containing acetonitrile, said second liquid storage bottle (12) is used for containing water, said third liquid storage bottle (8) is used for containing acetonitrile, said fourth liquid storage bottle (9) is used for containing water, and said fifth liquid storage bottle (10) is used for containing isopropanol.
3. The integrated pretreatment and analysis device for on-line detection of benzo (a) pyrene in hot-pressed vegetable oil according to claim 1, wherein said first chromatographic pump (1) is a ternary gradient pump or a quaternary gradient pump, and is used for respectively delivering acetonitrile in a third liquid storage bottle (8), water in a fourth liquid storage bottle (9) and isopropanol in a fifth liquid storage bottle (10); the second chromatographic pump (4) is a quaternary gradient pump and is used for respectively conveying acetonitrile in the first liquid storage bottle (11) and water in the second liquid storage bottle (12).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109959744A (en) * | 2019-04-25 | 2019-07-02 | 天津出入境检验检疫局动植物与食品检测中心 | The pre-treatment of benzo (a) pyrene and analysis integrated device and its detection method in on-line checking hot moulding vegetable oil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109959744A (en) * | 2019-04-25 | 2019-07-02 | 天津出入境检验检疫局动植物与食品检测中心 | The pre-treatment of benzo (a) pyrene and analysis integrated device and its detection method in on-line checking hot moulding vegetable oil |
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