CN103869014B - The extracting method of benzo (a) pyrene in a kind of edible oil - Google Patents
The extracting method of benzo (a) pyrene in a kind of edible oil Download PDFInfo
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- CN103869014B CN103869014B CN201410103856.1A CN201410103856A CN103869014B CN 103869014 B CN103869014 B CN 103869014B CN 201410103856 A CN201410103856 A CN 201410103856A CN 103869014 B CN103869014 B CN 103869014B
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Abstract
The present invention relates to benzo (a) pyrene pretreatment technology in edible oil, specifically disclose the extracting method of benzo (a) pyrene in a kind of edible oil, comprise the following steps: 1) get edible oil and carry out liquid-liquid extraction by the acetonitrile that normal hexane is saturated; 2) the raffinate fluid that previous step obtains is got, to described raffinate fluid re-extract operation; 3) merge the acetonitrile layer extract after each extraction, obtain total extract; 4) in total extract, add solid adsorbent, Separation of Solid and Liquid after purified treatment, gets supernatant; 5) supernatant is dried up under a nitrogen, heavy molten with acetonitrile, carry out liquid-phase chromatographic analysis after filtering membrane.The extraction operation steps of the present invention to benzo (a) pyrene is simple, economic and practical, impurity interference fully can be removed again while ensureing the recovery, improve detection sensitivity, reduce the maintenance of detecting instrument, increase the service life, be applicable to produce reality, be convenient to quick and precisely detect, there is good promotional value and application prospect.
Description
Technical field
The present invention relates to the pretreatment technology of benzo (a) pyrene, particularly relate to the extracting method of benzo (a) pyrene in a kind of edible oil, belong to food analysis field.
Background technology
Benzo (a) pyrene is palycyclic aromatic (PAHs) compound be made up of 5 phenyl ring, is a kind of strong carcinogen, may because of environmental pollution or starting material band people or to add man-hour temperature too high and produce in the process of producing vegetable oil.
At present, China detects in the up-to-date National Standard Method of Determination (GB/T22509-2008) of benzo (a) pyrene in vegetable oil and adopts aluminium oxide dress post, solid phase chromatography method carries out pre-treatment, also exist that the running time is long, reagent consumption is large, the recovery is unstable, to reagent and the problem such as personnel requirement is higher, so that can not effectively to detect fast residual the carrying out of benzo (a) pyrene in vegetable oil by this method well.The maximum limitation 2 μ g/kg of BaP in European Union's No. 208/2005 file regulation edible oil, Codex Alimentary Commission (CAC) specifies the maximum limitation 5 μ g/kg of BaP in edible oil and fat, GB2716-2005 edible vegetable oil hygienic standard specifies that the maximum limitation of China is 10 μ g/kg, to limit the quantity larger difference with the world.In March, 2010, namely Hunan Jinhao Camellia Oil Co., Ltd. of China (lower abbreviation Jin Hao company) etc. is found carcinogenic substance " benzopyrene " severe overweight, China strengthens the attention detected benzopyrene gradually, along with the concern of people's food security is strengthened day by day, there is stricter requirement to relevant detection.And one of the modal test item of mensuration Ze Shi Food Inspection mechanism of benzo (a) pyrene in vegetable oil, therefore set up one quick and precisely with science in reliable vegetable oil the detection method of benzo (a) pyrene content there is positive effect.
Affecting the principal element that in grease, benzo (a) pyrene measures is triglyceride a large amount of in grease and fatty accompaniment, and benzo (a) pyrene exists with trace level in edible oil, in extraction and purge process, easily further loss, affects testing result accuracy.Many organic compounds can be extracted out together with benzo (a) pyrene, and interference is further separated and quantitatively detects.The structure of a lot of PAHs is similar, makes the separation detection difficult of benzo (a) pyrene.At present, mensuration reversed-phased high performace liquid chromatographic two kinds of methods of benzo (a) pyrene mensuration and GB/T22509-2008 animal and plant fat benzo (a) pyrene in the National Standard Method of Determination GB/T5009.27-2003 food of benzo (a) pyrene in edible oil detect in China.National Standard Method of Determination GB/T5009.27-2003 adopts fluorescence spectrophotometry and visual colorimetry, comparatively large by such environmental effects, is vulnerable to external interference and produces error; In National Standard Method of Determination GB/T22509-2008, HPLC-fluorescence detection device method is simple and quick, but requires high to the neutral alumina of purification in method, and process is complicated, and the reappearance in practical operation and operability are not strong, complicated operation.
In recent years, also the pre-treating method of benzo (a) pyrene in other several detection edible oil and fat has been continued to bring out out, enumerate below and severally compare typical method: method one is hydrolyzed saponification, saponification can remove grease effectively, backflow saponification is carried out together with a certain amount of edible oil with the methyl alcohol of KOH or NaOH or ethanolic solution, after saponification 4h, not saponifiedly carry out gold-liquid extraction with cyclohexane etc. again, extract detects after concentrated; Method two gel permeation chromatography is separated.The method, based on the separation principle of size exclusion, utilizes each component molecular in sample to vary in size, thus in gel the hold-up time different and reach separation object.When gel permeation chromatography carries out purification separation to sample, first large molecule flows out, and isotope dilution method need be coordinated to adopt makings to detect; Method three Solid-Phase Extraction, is a kind of sample pretreatment technology based on liquid-solid separation extraction, purifies with solid phase extraction concentration.Dissolved by oil sample and extract, join in the solid-phase extraction column after activation, carry out gradient elution after enrichment, eluent detects after concentrated.Method four liquid-liquid extraction, by regulating the proportioning of different reagent, changing the dissolving distribution ratio of benzo (a) pyrene at grease and reagent, thus being isolated, detecting after concentrating.
Analysis for benzo (a) pyrene in edible oil measures, and pretreatment technology is very crucial.The fluorescence spectrophotometry detection limit adopted in benzo (a) pyrene bioassay standard in GB/T5009.27-2003 food is indefinite, just cannot reach the detection limit of 1ng/g when sample size deficiency or point sample quantity not sufficient; Visual colorimetry, can only carry out outline quantitatively, and these two kinds of methods is vulnerable to external interference.Adopt simple aluminium oxide decontaminating column decontamination substrate in the mensuration reversed-phased high performace liquid chromatographic standard of GB/T22509-2008 animal and plant fat benzo (a) pyrene, can flow out when the sampling amount of grease increases along with eluent, impact measures.
And for emerging several detection methods, being wherein hydrolyzed saponification method, length consuming time, saponification is not exclusively comparatively large to Influence on test result, causes sensitivity and accuracy to decline; In gel permeation chromatography, benzo (a) pyrene has good lipophilicity, and in elution process, competition binding causes the hold-up time indefinite, and size exclusion separating effect is bad, and after process, resid amount is many, and impact detects; Solid phase extraction requires strict to the filler of pillar, complicated for edible oil component, the composition of filler is not easily selected.Shown by a large amount of experiments simultaneously, a large amount of organic reagents can consumed with in solid phase extraction procedure, produce a large amount of waste liquids, be not easy to apply, and all have Residual oil with after different solid-phase extraction column wash-outs, there is impact to benzo (a) pyrene detection accuracy; Simple liquid-liquid extraction easily causes fat residue, reclaims the problems such as insufficient.The normal hexane that the employing acetonitrile mentioned in existing document is saturated dissolves, then adopt in benzo (a) the pyrene extracting method of the acetonitrile extraction that normal hexane is saturated, first the n-hexane dissolution edible oil that acetonitrile is saturated is adopted, this step grease removal effect is general, and two-phase is after certain proportion composite liberation, the normal hexane layer being dissolved with grease is in upper strata, be unfavorable for drawing and be separated, thus affect follow-up liquid phase detection, instrument is produced and pollutes, cause detection sensitivity low, instrument is short for serviceable life.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of method extracting benzo (a) pyrene from edible oil of improvement is provided.The technology of the present invention adopts the liquid-liquid extraction method optimized, acetonitrile extraction after adopting normal hexane saturated, benzo (a) pyrene is farthest separated with grease, adopt solid adsorbent simultaneously, reduce impurity interference, optimizing extracting process, meet benzo (a) pyrene and extract and require and the testing conditions of liquid phase, is the one quick and precisely extracting method of benzo (a) pyrene content in reliable vegetable oil with science.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: the extracting method of benzo (a) pyrene in a kind of edible oil, is characterized in that, comprise the following steps:
1) edible oil getting certain mass carries out liquid-liquid extraction, and extraction conditions is: using the saturated acetonitrile of normal hexane as extractant, and refrigerated centrifuge after the mixed concussion in whirlpool, is separated and obtains acetonitrile layer extract and raffinate fluid;
2) get the raffinate fluid that previous step obtains, described raffinate fluid is repeated to the extracting operation of step 1);
3) combining step 1) to 2) acetonitrile layer extract after each extraction, obtain total extract;
4) in total extract of previous step, add solid adsorbent, Separation of Solid and Liquid after purified treatment, gets supernatant;
5) supernatant of previous step is dried up under a nitrogen, heavy molten with acetonitrile, carry out liquid-phase chromatographic analysis after filtering membrane.
The invention has the beneficial effects as follows: the inventive method adopts the acetonitrile extraction and solid adsorbent purified treatment that normal hexane is saturated, utilizes high performance liquid chromatograph analysis, can complete the detection of benzo (a) pyrene in edible oil.Decrease the extraction running time of national standard method alumina column solid phase extraction, reagent consumption obviously reduces, and solid adsorbent reduces impurity interference, and protection instrument, increases the service life; Compare method for saponification, reduce the time of saponification backflow, operate simpler; For ultrasonic and gel permeation, there is more significantly effect of extracting, extract fast convenient.
On the basis of technique scheme, the present invention can also do following improvement.
Further, the mass volume ratio of edible oil and the saturated acetonitrile of extractant normal hexane is 1g:(8 ~ 10) ml.Extract consumption be chosen as prior art, the present invention is 1g:(8 ~ 10 for the angle Selection edible oil of economy and the mass volume ratio of extractant) mL.
Preferably, the time of step 1) mesoscale eddies concussion is 2 ~ 5min.
Preferred, the time of step 1) mesoscale eddies concussion is 2min.
Preferably, in step 1), the condition of refrigerated centrifuge is :-20 ± 2 DEG C, 3500 ~ 4000rpm, refrigerated centrifuge 10 ~ 15min.
Preferred, in step 1), the condition of refrigerated centrifuge is :-20 DEG C, 4000rpm, refrigerated centrifuge 15min.
Preferably, step 2) described multiplicity is 1 ~ 3 time.
Further, solid adsorbent described in step 4) is solid adsorbent SAX.
Preferably, the consumption of solid adsorbent described in step 4) is that every milliliter of total extract adds solid adsorbent 0.01 ~ 0.03g.
Preferably, the temperature that nitrogen described in step 5) dries up is 40 ~ 45 DEG C.
Preferred, the temperature that nitrogen described in step 5) dries up is 40 DEG C.
Preferably, the filtering membrane that step 5) adopts is 0.45 μm.
Preferably, the condition of liquid-phase chromatographic analysis described in step 5) is: analyze chromatographic column: palycyclic aromatic analytical column; Column temperature: 40 DEG C; Detecting device: FLD fluorescence detector, excitation wavelength 384nm, emission wavelength 416nm; Mobile phase is acetonitrile: water volume ratio is 90:10; Flow rate of mobile phase: 1mL/min; Sample size: 10 μ L.
The specification of described palycyclic aromatic analytical column is: column length 250mm, internal diameter 4.6mm, particle diameter 5 μm.
Second aspect present invention discloses the application of aforementioned extracting method in edible oil in benzo (a) pyrene content detection.
The beneficial effect of above-mentioned further scheme is adopted to be, the present invention adopts the acetonitrile extraction that reagent normal hexane is saturated, make benzo (a) pyrene be farthest dissolved into acetonitrile mutually in, reduce fat residue, and with solid adsorbent SAX adsorbing contaminant, replace alumina column, reduce the step of dress post and activation, easy to operation, national standard method detectability can be reached simultaneously, have good sensitivity and accuracy.
This method passes through Optimal improvements, centrifugal process after extraction is adopted refrigerated centrifuge, utilize the characteristic that oil at low temperature solidifies, reach and reduce extract Residual oil, add solid adsorbent SAX simultaneously, by the fully absorption such as the pigment of complicated component, fatty acid, the pollution to chromatographic column can be reduced, improve the object of detection sensitivity.
The inventive method adopts the acetonitrile extraction and solid adsorbent purified treatment that normal hexane is saturated, utilizes high performance liquid chromatograph analysis, can complete the detection of benzo (a) pyrene in edible oil.Compared with the mensuration reversed-phased high performace liquid chromatographic standard method of GB GB/T22509-2008 animal and plant fat benzo (a) pyrene adopted with current most testing agency:
(1) this invention technical operation step is simple and quick, reduce aluminum oxide activating, dress post, cross post process, operation is simple, and experimental period can be completed by several hours by original one to two days time decreased, be convenient to grasp testing result fast, significant to production control.
(2) national standard method consumes amount of reagent greatly, the organic reagent of activation, flushing process at substantial, and this invention technology reagent dosage is few, economic and practical, can reduce harm and the exhaust emission of organic reagent simultaneously.
(3) the method adopts refrigerated centrifuge, effective removal Residual oil, 40 DEG C of nitrogen blow and keep benzo (a) pyrene characteristic, testing result can be made to stablize, adopt solid adsorbent SAX fully can remove again impurity interference, improve detection sensitivity, reduce the maintenance of detecting instrument, extend instrument serviceable life.
The extraction operation steps of the present invention to benzo (a) pyrene is simple, economic and practical in sum, impurity interference fully can be removed again while ensureing the recovery, improve detection sensitivity, reduce the maintenance of detecting instrument, increase the service life, be applicable to produce reality, be convenient to quick and precisely detect, there is good promotional value and application prospect.
Accompanying drawing explanation
Fig. 1 is the HPLC collection of illustrative plates that in peanut oil, benzo (a) pyrene detects;
Fig. 2 is the HPLC collection of illustrative plates that in corn oil, benzo (a) pyrene detects.
Embodiment
Be described principle of the present invention and feature below in conjunction with accompanying drawing, example, only for explaining the present invention, is not intended to limit scope of the present invention.
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.
Embodiment 1
Accurately take one-level squeezing peanut oil 0.5g(and be accurate to 0.001g) in 15mL nut plastic centrifuge tube, add the acetonitrile that 4mL normal hexane is saturated, whirlpool concussion 5min,-18 DEG C of refrigerated centrifuges, 3500rpm, centrifugal 15min, be transferred to acetonitrile layer in another clean plastic tube.Repeat extraction 2 times, merge acetonitrile layer, be extract.
Solid adsorbent SAX0.2g is added in extract (10ml), whirlpool concussion 2min, 3000rpm, centrifugal 5min, upper strata scavenging solution is shifted out and blows to dry in 40 DEG C of nitrogen, add 1mL acetonitrile heavy molten, cross 0.45 μm of organic filter membrane, detect for liquid phase, the condition that liquid phase detects is: analyze chromatographic column: palycyclic aromatic analytical column, column length 250mm, internal diameter 4.6mm, particle diameter 5 μm; Column temperature: 40 DEG C; Detecting device: FLD fluorescence detector, excitation wavelength 384nm, emission wavelength 416nm; Mobile phase: 90% acetonitrile-10% water; Flow rate of mobile phase: 1mL/min; Sample size: 10 μ L.Accompanying drawing 1 is shown in by HPLC collection of illustrative plates, and testing result is 1.5 μ g/kg.
Embodiment 2
Accurately take one-level corn oil 0.5g(and be accurate to 0.001g) in 15mL nut plastic centrifuge tube, add the acetonitrile that 5mL normal hexane is saturated, whirlpool concussion 2min,-22 DEG C of refrigerated centrifuges, 4000rpm, centrifugal 10min, be transferred to acetonitrile layer in another clean plastic tube.Repeat extraction 3 times, merge the acetonitrile layer extracted for three times, be extract.
Solid adsorbent SAX0.3g is added, whirlpool concussion 2min, 3000rpm in extract (10ml), centrifugal 3min, upper strata scavenging solution shifted out and blows to dry in 45 DEG C of nitrogen, adding 1mL acetonitrile heavy molten, cross 0.45 μm of organic filter membrane, detect for liquid phase,, the condition that liquid phase detects is: analyze chromatographic column: palycyclic aromatic analytical column, column length 250mm, internal diameter 4.6mm, particle diameter 5 μm; Column temperature: 40 DEG C; Detecting device: FLD fluorescence detector, excitation wavelength 384nm, emission wavelength 416nm; Mobile phase: 90% acetonitrile-10% water; Flow rate of mobile phase: 1mL/min; Sample size: 10 μ L.Accompanying drawing 2 is shown in by HPLC collection of illustrative plates, and testing result is 0.75 μ g/kg.
Claims (9)
1. the extracting method of benzo (a) pyrene in edible oil, is characterized in that, comprise the following steps:
1) edible oil getting certain mass carries out liquid-liquid extraction, and extraction conditions is: using the saturated acetonitrile of normal hexane as extractant, and refrigerated centrifuge after the mixed concussion in whirlpool, is separated and obtains acetonitrile layer extract and raffinate fluid;
2) get the raffinate fluid that previous step obtains, step 1 repeated to described raffinate fluid) extracting operation;
3) combining step 1) to 2) acetonitrile layer extract after each extraction, obtain total extract;
4) in total extract of previous step, add solid adsorbent, Separation of Solid and Liquid after purified treatment, gets supernatant, and described solid adsorbent is solid adsorbent SAX;
5) supernatant of previous step is dried up under a nitrogen, heavy molten with acetonitrile, to carrying out liquid-phase chromatographic analysis after filtering membrane.
2. extracting method as claimed in claim 1, is characterized in that, step 1) mass volume ratio of described edible oil and the saturated acetonitrile of extractant normal hexane is 1g:8 ~ 10mL.
3. extracting method as claimed in claim 1, is characterized in that, step 1) in the condition of refrigerated centrifuge be :-20 ± 2 DEG C, 3500 ~ 4000rpm, refrigerated centrifuge 10 ~ 15min.
4. extracting method as claimed in claim 1, is characterized in that, step 2) described multiplicity is 1 ~ 3 time.
5. extracting method as claimed in claim 1, is characterized in that, step 4) consumption of described solid adsorbent is that every milliliter of total extract adds solid adsorbent 0.01 ~ 0.03g.
6. extracting method as claimed in claim 1, is characterized in that, step 5) temperature that dries up of described nitrogen is 40 ~ 45 DEG C.
7. extracting method as claimed in claim 1, is characterized in that, step 5) filtering membrane that adopts is 0.45 μm.
8. extracting method as claimed in claim 1, is characterized in that, step 5) condition of described liquid-phase chromatographic analysis is: analyze chromatographic column: palycyclic aromatic analytical column; Column temperature: 40 DEG C; Detecting device: FLD fluorescence detector, excitation wavelength 384nm, emission wavelength 416nm; Mobile phase is acetonitrile: water volume ratio is 90:10; Flow rate of mobile phase: 1mL/min; Sample size: 10 μ L.
9. the application of extracting method in edible oil in benzo (a) pyrene content detection described in the arbitrary claim of claim 1-8.
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104403681A (en) * | 2014-11-26 | 2015-03-11 | 辽宁石油化工大学 | Method for extracting benzopyrene from coal pitch |
| CN104569193A (en) * | 2014-12-29 | 2015-04-29 | 山东龙大粮油有限公司 | Detection method of polycyclic aromatic hydrocarbon in edible oil |
| CN105203373A (en) * | 2015-09-10 | 2015-12-30 | 上海安谱实验科技股份有限公司 | Method for simply, fast, efficiently and stably testing benzopyrene in food |
| CN105223301A (en) * | 2015-09-23 | 2016-01-06 | 成都艾比科生物科技有限公司 | A kind of method for measuring benzopyrene content in vegetable oil |
| CN106280542B (en) * | 2016-08-15 | 2017-11-17 | 晨光生物科技集团股份有限公司 | A kind of production method for improving lycopene oleoresin quality |
| CN106556657A (en) * | 2016-11-03 | 2017-04-05 | 山东三星玉米产业科技有限公司 | The detection method of benzopyrene in Semen Maydis oil |
| CN106501411A (en) * | 2016-11-04 | 2017-03-15 | 无锡艾科瑞思产品设计与研究有限公司 | A kind of method for quick of benzopyrene from edible oil |
| CN107607657A (en) * | 2017-09-26 | 2018-01-19 | 山东龙大粮油有限公司 | The liquid chromatography detecting method of polycyclic aromatic hydrocarbon in a kind of edible oil |
| CN109580318A (en) * | 2018-12-11 | 2019-04-05 | 江南大学 | A kind of method of distributing Solid Phase Extraction processing edible oil sample detection benzo [a] pyrene |
| CN110045047A (en) * | 2019-05-23 | 2019-07-23 | 开化县检验检测研究院 | A kind of method of liquid-liquid micro-extraction processing edible vegetable oil sample detection benzo [a] pyrene |
| CN110389223A (en) * | 2019-07-25 | 2019-10-29 | 广东省食品检验所(广东省酒类检测中心) | A kind of colloidal gold immunity chromatography quickly measuring benzo (α) pyrene in edible oil |
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| WO2004102181A2 (en) * | 2003-05-13 | 2004-11-25 | Cargill, Incorporated | Determination of aromatic hydrocarbons in edible oil products |
| CN102288720A (en) * | 2011-07-26 | 2011-12-21 | 中国林业科学研究院亚热带林业研究所 | Method for detecting benzo(a)pyrene of oiltea camellia seed oil |
| CN103472170A (en) * | 2013-09-10 | 2013-12-25 | 遵义市产品质量检验检测院 | Method for detecting benzopyrene in edible oil |
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