CN110045047A - A kind of method of liquid-liquid micro-extraction processing edible vegetable oil sample detection benzo [a] pyrene - Google Patents
A kind of method of liquid-liquid micro-extraction processing edible vegetable oil sample detection benzo [a] pyrene Download PDFInfo
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- CN110045047A CN110045047A CN201910432621.XA CN201910432621A CN110045047A CN 110045047 A CN110045047 A CN 110045047A CN 201910432621 A CN201910432621 A CN 201910432621A CN 110045047 A CN110045047 A CN 110045047A
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
Abstract
The invention discloses a kind of methods of liquid-liquid micro-extraction processing edible vegetable oil sample detection benzo [a] pyrene, using dehydroactic acid/acetonitrile mixed organic solvents as benzo [a] pyrene extractant, high performance liquid chromatography detection can be carried out by being extracted twice rear extract liquor to edible vegetable oil pre-treatment, the content of benzo [a] pyrene in you can get it food plant oil samples is calculated by conversion, compare the pre-treatments extractants such as conventional hexamethylene, sample recovery rate greatly improves, have the advantages that extraction efficiency is high, Solvent quantity is few, concentration process is blown without revolving or nitrogen, it is easy to operate, step is few, it is time-consuming short.
Description
Technical field
The present invention relates to edible oil detection technique field, in particular to a kind of liquid-liquid micro-extraction handles food plant oil samples
The method for detecting benzo [a] pyrene.
Background technique
Benzo [a] pyrene is not soluble in water, is soluble in chloroform, benzene, acetone and other organic solvent, is that a kind of common high activity is indirect
Carcinogenic substance and Mutagen, and it is confirmed to be that a kind of strongest compound of carcinogenicity in polycyclic aromatic hydrocarbon is current, measurement benzo [a] pyrene
Main method has liquid chromatogram-fluorescence detection and gas chromatography-mass spectrography etc..Used Sample Pretreatment Technique before sample introduction
Mainly liquid-liquid extraction, Solid Phase Extraction, ultrasonic extraction, accelerated solvent extraction etc., but there is cumbersome, at high cost, easy band
The disadvantages of carrying out secondary pollution.Dispersive liquid-liquid microextraction (DLLME) is a kind of environmentally friendly new technology, due to easy to operate, is disappeared
It is few to consume organic solvent, and does not need special price apparatus, it is combined measurement food with analysis instrument by many researchers
Pesticide residue and hormone pollutant in product and environmental water sample, and using dispersive liquid-liquid microextraction as changing in edible oil sample
The report for learning the pre-treating method of substance detection is actually rare.
Pi-pi accumulation be aromatic compound a kind of special space arrangement, refer to it is a kind of occur often in it is weak between aromatic rings
Interaction is typically found between opposite electron rich and two molecules of electron deficient, is a kind of non-with hydrogen bond no less important
Covalent bond interaction.
Currently, the general technology scheme of liquid-liquid extraction method is general are as follows: 1, weigh a certain amount of sample, fluid sample can directly into
Row extraction, solid sample needs are dispersed with agent is extracted；2, extractant is added to be extracted, it is general extract twice or repeatedly
It takes；3, merge extractant and carry out revolving or nitrogen blow concentration；4, it is redissolved, is measured with suitable solvent.And liquid-liquid extraction method exists
Come with some shortcomings place in the application of edible vegetable oil detection benzo [a] pyrene, mainly has the following aspects: 1, selected solvent
Extraction yield is lower, needs repeatedly to extract；2, the consumption of extractant is relatively more；3, nitrogen is needed to blow or rotate, cumbersome, consumption
Duration.
Summary of the invention
The technical problems to be solved by the invention: this technology invention is primarily to solve liquid-liquid extraction in edible vegetable oil
Method measure benzo [a] pyrene during existing shortcoming, main target be develop a kind of consumption extractant it is few, it is easy,
The method of benzo [a] pyrene is measured in quick edible vegetable oil.
In order to solve the above technical problems, the present invention provides technical solution below:
A kind of method of liquid-liquid micro-extraction processing edible vegetable oil sample detection benzo [a] pyrene, includes following specific steps:
(1) weigh sample: food plant oil samples sample weighting amount is 0.0500~0.1500g；
(2) sample pre-treatments: weighed food plant oil samples are placed in 1.5mL centrifuge tube, and 0.5~1.5mL is added
Dehydroactic acid/acetonitrile extraction agent is put into 35 DEG C of pre-set constant-temperature ultrasonic water-baths after the concussion that is vortexed mixes, ultrasound
After be centrifuged, take out sample be sucked out upper layer of extraction liquid 0.5~1.5mL dehydrogenation is added in 5mL centrifuge tube, in lower liquid
Acetic acid/acetonitrile extraction agent repeats extraction once, and the merging of upper layer of extraction liquid twice is placed in same centrifuge tube, is mixed well
Obtain HPLC loading sample；The dehydroactic acid/acetonitrile extraction agent is the mixture of acetonitrile and dehydroactic acid；
(3) HPLC loading sample is measured into benzo [a] pyrene content using stationary phases for HPLC, is scaled edible plant
Benzo [a] pyrene content in object oil.
Preferably, the dehydroactic acid/acetonitrile extraction agent is added dehydroactic acid to after being saturated, is used using acetonitrile as solvent
The extraction of benzo [a] pyrene in edible vegetable oil.
Preferably, it is 500~800W, 5~10min of ultrasonic time that the ultrasonic power is constant；The centrifugally operated is
3~5min is centrifuged under 6500~8000rpm speed.
Preferably, the method for described liquid-liquid micro-extraction processing edible vegetable oil sample detection benzo [a] pyrene is with three times noise
Than for method detection limit, detection is limited to 0.2 μ g/kg；Using ten times of signal-to-noise ratio as method quantitative limit, it is quantitatively limited to 0.5 μ g/kg.
Preferably, additional amount of the dehydroactic acid/acetonitrile extraction agent in extraction twice is identical, in food plant oil sample
When product sample weighting amount is 0.1000g, additional amount is 1.00mL extractant.
Preferably, the stationary phases for HPLC determination condition is as follows:
Chromatographic column: C8, column length 250mm, internal diameter 4.6mm, 5 μm of partial size；
Mobile phase: acetonitrile+water=88%+12%；
Flow velocity: 1.0mL/min；
Fluorescence detector: excitation wavelength 384nm, launch wavelength 406nm；
Column temperature: 30 DEG C；
Single sample volume: 20 μ L.
It is that the present invention obtains the utility model has the advantages that
Have the advantages that extraction efficiency is high using dehydroactic acid/acetonitrile mixed organic solvents as benzo [a] pyrene extractant,
Solvent quantity is few, and be available on the machine measurement after ultrasonic wave added micro-extraction twice, blows concentration process without revolving or nitrogen, grasps
Make simplicity, step is few, time-consuming short.
Detailed description of the invention:
Fig. 1 benzo [a] pyrene standard curve；
Fig. 2 benzo [a] pyrene standard substance chromatogram；
Benzo [a] pyrene sample chromatogram figure in Fig. 3 embodiment 3.
Specific embodiment
Below by the description to embodiment, specific embodiments of the present invention will be described in further detail, with side
Those skilled in the art is helped to have more complete, accurate and deep understanding to inventive concept of the invention, technical solution.
Embodiment 1:
One, reagent prepare and it is prefabricated
Dehydroactic acid/acetonitrile extraction agent is the mixture of acetonitrile and dehydroactic acid, and acetonitrile is as solvent, and dehydroactic acid is in second
Concentration in nitrile is 0.10g/mL；Dehydroactic acid has more pi bond, can have preferable pi-pi accumulation phase interaction with benzo [a] pyrene
With noncovalent intermolecular interactions are obvious, and affinity is high, therefore, can be dissolved in dehydroactic acid in acetonitrile to benzo [a] pyrene
Carry out liquid-liquid micro-extraction.
Two, edible vegetable oil sample detection benzo [a] pyrene is handled using liquid-liquid micro-extraction, includes following specific steps:
(1) weigh sample: currently invention addresses the methods of liquid-liquid micro-extraction, using three times signal-to-noise ratio as method detection limit, inspection
Rising limit is 0.2 μ g/kg；Using ten times of signal-to-noise ratio as method quantitative limit, it is quantitatively limited to 0.5 μ g/kg, comprehensively considers benzo [a] pyrene
Food plant oil samples sample weighting amount is determined as 0.0500g by the dilution volume of instrument detection limit and sample；
(2) sample pre-treatments: weighed food plant oil samples are placed in 1.5mL centrifuge tube, and 0.5mL dehydrogenation second is added
Acid/acetonitrile extraction agent is put into 35 DEG C of pre-set constant-temperature ultrasonic water-baths after the concussion that is vortexed mixes, and ultrasonic power is permanent
It is set to 500W, ultrasonic time 5min；It is centrifuged after ultrasound, centrifugally operated is to be centrifuged 3min under 6500rpm speed.Take out sample
Suction upper layer of extraction liquid adds 1.5mL dehydroactic acid/acetonitrile extraction agent in 5mL centrifuge tube, in lower liquid and repeats extraction
It takes once, the merging of upper layer of extraction liquid twice is placed in same centrifuge tube, HPLC loading sample is mixed well to obtain；
(3) HPLC loading sample is measured into benzo [a] pyrene content, high performance liquid chromatography using stationary phases for HPLC
Fluorescence measurement fixed condition is as follows:
Chromatographic column: C8, column length 250mm, internal diameter 4.6mm, 5 μm of partial size；
Mobile phase: acetonitrile+water=88%+12%；
Flow velocity: 1.0mL/min；
Fluorescence detector: excitation wavelength 384nm, launch wavelength 406nm；
Column temperature: 30 DEG C；
Single sample volume: 20 μ L.
(4) by the way that benzo [a] pyrene content in HPLC loading sample is scaled the benzo [a] in food plant oil samples
Pyrene content.
Embodiment 2:
One, reagent prepare and it is prefabricated
Dehydroactic acid/acetonitrile extraction agent is the mixture of acetonitrile and dehydroactic acid, and acetonitrile is as solvent, and dehydroactic acid is in second
Concentration in nitrile is 0.08g/mL；
Two, edible vegetable oil sample detection benzo [a] pyrene is handled using liquid-liquid micro-extraction, includes following specific steps:
(1) weigh sample: currently invention addresses the methods of liquid-liquid micro-extraction, using three times signal-to-noise ratio as method detection limit, inspection
Rising limit is 0.2 μ g/kg；Using ten times of signal-to-noise ratio as method quantitative limit, it is quantitatively limited to 0.5 μ g/kg, comprehensively considers benzo [a] pyrene
Food plant oil samples sample weighting amount is determined as 0.1500g by the dilution volume of instrument detection limit and sample；
(2) sample pre-treatments: weighed food plant oil samples are placed in 2mL centrifuge tube, and 1.5mL dehydrogenation second is added
Acid/acetonitrile extraction agent is put into 35 DEG C of pre-set constant-temperature ultrasonic water-baths after the concussion that is vortexed mixes, and ultrasonic power is permanent
It is set to 800W, ultrasonic time 10min；It is centrifuged after ultrasound, centrifugally operated is to be centrifuged 5min under 8000rpm speed.Take out sample
Product suction upper layer of extraction liquid adds 0.5mL dehydroactic acid/acetonitrile extraction agent in 5mL centrifuge tube, in lower liquid and repeats
Extraction is primary, and upper layer of extraction liquid merging twice is placed in same centrifuge tube, HPLC loading sample is mixed well to obtain；
(3) HPLC loading sample is measured into benzo [a] pyrene content, high performance liquid chromatography using stationary phases for HPLC
Fluorescence measurement fixed condition is as follows:
Chromatographic column: C8, column length 250mm, internal diameter 4.6mm, 5 μm of partial size；
Mobile phase: acetonitrile+water=88%+12%；
Flow velocity: 1.0mL/min；
Fluorescence detector: excitation wavelength 384nm, launch wavelength 406nm；
Column temperature: 30 DEG C；
Single sample volume: 20 μ L.
(4) by the way that benzo [a] pyrene content in HPLC loading sample is scaled the benzo [a] in food plant oil samples
Pyrene content.
Embodiment 3:
One, reagent prepare and it is prefabricated
Dehydroactic acid/acetonitrile extraction agent is added excessive dehydroactic acid to after being saturated, supernatant is taken to be used for using acetonitrile as solvent
The extraction of benzo [a] pyrene in edible vegetable oil.
Two, edible vegetable oil sample detection benzo [a] pyrene is handled using liquid-liquid micro-extraction, includes following specific steps:
(1) weigh sample: currently invention addresses the methods of liquid-liquid micro-extraction, using three times signal-to-noise ratio as method detection limit, inspection
Rising limit is 0.2 μ g/kg；Using ten times of signal-to-noise ratio as method quantitative limit, it is quantitatively limited to 0.5 μ g/kg, comprehensively considers benzo [a] pyrene
Food plant oil samples sample weighting amount is determined as 0.1000g by the dilution volume of instrument detection limit and sample；
(2) sample pre-treatments: weighed food plant oil samples are placed in 1.5mL centrifuge tube, and 1.00mL dehydrogenation is added
Acetic acid/acetonitrile extraction agent is put into 35 DEG C of pre-set constant-temperature ultrasonic water-baths, ultrasonic power after the concussion that is vortexed mixes
Constant is 650W, ultrasonic time 7min；It is centrifuged after ultrasound, centrifugally operated is to be centrifuged 4min under 7500rpm speed.Take out sample
Product suction upper layer of extraction liquid adds 1.00mL dehydroactic acid/acetonitrile extraction agent in 5mL centrifuge tube, in lower liquid and repeats
Extraction is primary, and upper layer of extraction liquid merging twice is placed in same centrifuge tube, HPLC loading sample is mixed well to obtain；
(3) HPLC loading sample is measured into benzo [a] pyrene content, high performance liquid chromatography using stationary phases for HPLC
Fluorescence measurement fixed condition is as follows:
Chromatographic column: C8, column length 250mm, internal diameter 4.6mm, 5 μm of partial size；
Mobile phase: acetonitrile+water=88%+12%；
Flow velocity: 1.0mL/min；
Fluorescence detector: excitation wavelength 384nm, launch wavelength 406nm；
Column temperature: 30 DEG C；
Single sample volume: 20 μ L.
(4) by the way that benzo [a] pyrene content in HPLC loading sample is scaled the benzo [a] in food plant oil samples
Pyrene content.
Comparative examples 1: according to document: Peng little Dong, Wang Huan, Li Hongzhou wait liquid-phase extraction-reversed-phase high performance liquid chromatography
BaP [J] Chinese oil in method combination measurement vegetable oil, 2018,43 (10): the method that 119-121. is provided measures different
The rate of recovery of benzo [a] pyrene under extractant pre-treatment.
Regulation enforcement embodiment 3 and comparative examples 1 are controlled using GB 27404-2008 Good Laboratory, measurement is edible
The recovery of standard addition of benzo [a] pyrene in ready-mixed oil: single loading benzo [a] pyrene mark-on sample chromatogram figure is shown in Fig. 3.
The preparation of benzo [a] pyrene (BaP) standard reserving solution and standard solution:
Accurate 100 μ g/mL benzo [a] the pyrene standard substance 1.00mL that draw are in 10mL volumetric flask, with chromatography acetonitrile constant volume,
Obtain 10 μ g/mL benzo [a] pyrene standard reserving solutions, carry out gradient dilution step by step with chromatography acetonitrile, obtain 0.02,0.05,0.1,
0.5,1.0 μ g/L standard working solution.HPLC detection benzo [a] pyrene standard substance chromatogram is shown in Fig. 2；
With benzo [a] pyrene standard working solution mass concentration (x) for abscissa, peak area (y) is that ordinate draws standard song
Line, benzo [a] pyrene standard curve are shown in Fig. 1.As shown in Figure 1, benzo [a] pyrene is in 0.02~1.0 μ g/L mass concentration range interior lines
Good, the regression equation of property: Y=1.55 × 106X+1.06×104, correlation coefficient r=0.999924 (see Fig. 1)；
Peak area value in benzo [a] pyrene mark-on HPLC loading sample chromatogram figure is substituted into the standard curve obtained by Fig. 1
In, mark-on benzo [a] pyrene content is calculated, the BaP concentration and recovery of standard addition in different HPLC loading samples are calculated, is calculated public
Formula:
The calculating of benzo [a] pyrene content sees below formula in edible oil sample:
In formula: A is the measurement content of benzo [a] pyrene in edible oil sample, μ g/kg；C is on the quantitative HPLC of standard curve
All product benzo [a] pyrene mass concentrations, μ g/L；V is HPLC loading sample constant volume, mL；M is sample quality, g；D is dilution
Multiple, no dilution d=1.
The rate of recovery is calculated as follows:
A0Content, μ g/kg are measured for benzo [a] pyrene of blank；A is the measurement content of benzo [a] pyrene in edible oil sample,
μg/kg；
Measurement and calculated result are shown in Table 1:
1 embodiment 3 of table measures the recovery of standard addition result of benzo [a] pyrene (BaP) in edible blend oil
It is compared as solvent, using pure acetonitrile as pre-treatment extractant, measures mark-on reclaims according to said determination method
Rate the results are shown in Table 2:
The acetonitrile extraction agent recovery of standard addition result of benzo [a] pyrene in 2 edible blend oil of table
It is found that the present invention is using saturation dehydroactic acid acetonitrile after the Comparative result of 1 result of table and comparative examples 1 and table 2
Solution as extractant, to the effect of extracting of benzo [a] pyrene be significantly higher than hexamethylene or acetonitrile etc. other it is a variety of commonly use it is organic molten
Agent, final sample recovery rate are significantly higher than other pre-treatment liquid phase extractants, have given full play to liquid-liquid micro-extraction edible
Advantage in oily benzo [a] pyrene detection.
The rate of recovery is higher than 100% and belongs to normal instrument detection and calculate in error range, the evaluated error with background values
Correlation does not influence high effect of extracting identification of the invention.
In conclusion having extraction efficiency using dehydroactic acid/acetonitrile mixed organic solvents as benzo [a] pyrene extractant
High advantage, Solvent quantity is few, and be available on the machine measurement after ultrasonic wave added micro-extraction twice, blows without revolving or nitrogen dense
Compression process, easy to operate, step is few, time-consuming short.
The above examples only illustrate the technical idea of the present invention, and this does not limit the scope of protection of the present invention, all
According to the technical idea provided by the invention, any changes made on the basis of the technical scheme each falls within the scope of the present invention
Within；The technology that the present invention is not directed to can be realized by the prior art.
Claims (6)
1. a kind of method of liquid-liquid micro-extraction processing edible vegetable oil sample detection benzo [a] pyrene, which is characterized in that comprising as follows
Specific steps:
(1) weigh sample: food plant oil samples sample weighting amount is 0.0500~0.1500g；
(2) sample pre-treatments: weighed food plant oil samples are placed in 1.5mL centrifuge tube, and 0.5~1.5mL dehydrogenation is added
Acetic acid/acetonitrile extraction agent is put into 35 DEG C of pre-set constant-temperature ultrasonic water-baths, ultrasound finishes after the concussion that is vortexed mixes
After be centrifuged, take out sample be sucked out upper layer of extraction liquid 0.5~1.5mL dehydrogenation second is added in 5mL centrifuge tube, in lower liquid
Acid/acetonitrile extraction agent repeats extraction once, and the merging of upper layer of extraction liquid twice is placed in same centrifuge tube, is mixed well
HPLC loading sample；The dehydroactic acid/acetonitrile extraction agent is the mixture of acetonitrile and dehydroactic acid；
(3) HPLC loading sample is measured into benzo [a] pyrene content using stationary phases for HPLC, is scaled edible vegetable oil
In benzo [a] pyrene content.
2. a kind of side of liquid-liquid micro-extraction processing edible vegetable oil sample detection benzo [a] pyrene according to claim 1
Method, it is characterised in that: the dehydroactic acid/acetonitrile extraction agent is added dehydroactic acid to after being saturated, is used for using acetonitrile as solvent
The extraction of benzo [a] pyrene in edible vegetable oil.
3. a kind of side of liquid-liquid micro-extraction processing edible vegetable oil sample detection benzo [a] pyrene according to claim 1
Method, it is characterised in that: the constant ultrasonic power is 500~800W, 5~10min of ultrasonic time；The centrifugally operated is 6500
3~5min is centrifuged under~8000rpm speed.
4. a kind of side of liquid-liquid micro-extraction processing edible vegetable oil sample detection benzo [a] pyrene according to claim 1
Method, it is characterised in that: the method for described liquid-liquid micro-extraction processing edible vegetable oil sample detection benzo [a] pyrene is with three times signal-to-noise ratio
For method detection limit, detection is limited to 0.2 μ g/kg；Using ten times of signal-to-noise ratio as method quantitative limit, it is quantitatively limited to 0.5 μ g/kg.
5. a kind of side of liquid-liquid micro-extraction processing edible vegetable oil sample detection benzo [a] pyrene according to claim 1
Method, it is characterised in that: additional amount of the dehydroactic acid/acetonitrile extraction agent in extraction twice is identical, in food plant oil sample
When product sample weighting amount is 0.1000g, additional amount is 1.00mL extractant.
6. a kind of side of liquid-liquid micro-extraction processing edible vegetable oil sample detection benzo [a] pyrene according to claim 1
Method, it is characterised in that: the stationary phases for HPLC determination condition is as follows:
Chromatographic column: C8, column length 250mm, internal diameter 4.6mm, 5 μm of partial size；
Mobile phase: acetonitrile+water=88%+12%；
Flow velocity: 1.0mL/min；
Fluorescence detector: excitation wavelength 384nm, launch wavelength 406nm；
Column temperature: 30 DEG C；
Single sample volume: 20 μ L.
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| CN201911017282.5A CN110715993B (en) | 2019-05-23 | 2019-10-24 | Method for detecting benzo [ a ] pyrene by liquid-liquid micro-preparation treatment of edible vegetable oil sample |
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| CN102072893B (en) * | 2010-12-16 | 2012-05-23 | 厦门大学 | Fluorescent detection method of benzo (a) pyrene in edible oil |
| CN103869014B (en) * | 2014-03-19 | 2015-09-23 | 山东鲁花集团有限公司 | The extracting method of benzo (a) pyrene in a kind of edible oil |
| CN105866288A (en) * | 2016-05-10 | 2016-08-17 | 芜湖雨耕山食品检测有限公司 | Method of utilizing high performance liquid chromatography to detect benzo (a) pyrene in edible oil |
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