CN104458939B - A kind of Camellia nitidissima oils volatile ingredient detection method - Google Patents
A kind of Camellia nitidissima oils volatile ingredient detection method Download PDFInfo
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Abstract
The present invention relates to organophosphorous pesticides-mass spectrometric hyphenated technique field, a kind of Camellia nitidissima oils volatile ingredient detection method is provided, comprise that SPE absorption-gas chromatography-mass spectrography detects, described SPE is the extraction of head space stirring rod solid phase adsorption, and described stirring rod scribbles based on two dimension or three-dimensional graphene-polymer coating. The material of described graphene-polymer coating comprise Graphene and Graphene material modified, described Graphene is material modified comprises graphene oxide, Graphene-polyethylene glycol dimethacrylate, graphene-polypyrrole, Graphene-poly-MTMS and Graphene class nano material. Camellia nitidissima oils volatile ingredient detection method of the present invention have detect accurate, highly sensitive, selective absorption is effective and the feature of long service life.
Description
Technical field
The present invention relates to organophosphorous pesticides-mass spectrometric hyphenated technique field, particularly a kind of detection method that is applied in Camellia nitidissima oils volatile ingredient.
Background technology
Camellia nitidissima belongs to Theaceae, Camellia, with tea, camellia, South Mountain tea, oil tea, tea plum etc. be twin sisters. Camellia nitidissima spend golden yellow, dazzling brilliant, be coated with seemingly coating of wax, sparkling and crystal-clear and glossy, seemingly have translucent sense. Camellia nitidissima is singly born in axil, when the flowers are in blossom, have cup-shaped, gyalectiform or bowl-shape, delicate and charming colourful, beautiful grace. In the past, people did not see the golden yellow kind of pattern. Nineteen sixty, Chinese science worker has found a kind of flavous camellia at Nanning one band first, is named as Camellia nitidissima. Being referred to as magical " Dongfang " magic tea abroad, being described as " plant kingdom giant panda ", " queen of tea family ", is one of eight kinds of first class of protection plants of country, and the ground such as MeiZhou,GuangDong, Guangxi Fangcheng Port also have manually and introduce a fine variety.
About Camellia nitidissima, Compendium of Material Medica has carries: " camellia produces south ... have again the names such as a sth. made by twisting is red, and Chiba is red, Chiba is white, or cloud also has yellow person "; Guangxi " local chronicle " is also on the books: " Camellia nitidissima, evergreen shrubs are grown in barren hill "; " Ye Hehua of Camellia nitidissima, through processing can do famous and precious heat-clearing, control dysentery, fat removing and decompression ". Among the people in area, Guangdong and Guangxi Provinces, the Camellia nitidissima of common people's extensive use over the past thousands of years make tea or Baoshang with clearing heat and detoxicating, blood lipid-reducing blood sugar-decreasing, diuresis are dried, step-down and improve immunity etc.
Research is found, golden camellia tea and spend in be rich in Tea Polyphenols, cupreol, the trace elements such as the active skull cap components such as anthocyanidin, general flavone (isoflavones, biflavone, flavanols, chalcone, aurones, anthocyanin, two hydrogen Huang (alcohol) and neoflavonoid etc.), several amino acids, oleanolic acid, soluble sugar, natural VE, 18 carbonic acid, phthalic acid list (ethylhexyl) ester, Kaempferol and selenium, manganese, iron, zinc.
In the composition of Camellia nitidissima, oiliness volatile ingredient mainly comprises arbricolin, 1,2-epoxy octadecane, 1,2-Disparmone, irisone, phytol, linoleic acid, methyl linoleate, ethyl linoleate etc., such oiliness volatile ingredient has the effects such as nti-freckle, desalination scar and striae of pregnancy, has application prospect very widely.
Because oiliness volatile ingredient content in Camellia nitidissima is lower, existing research concentrates on the higher Camellia nitidissima active component of some content abundance mostly as separation context of detection such as camellia chrysantha polysaccharide, Tea Polyphenols, general flavones, and the oiliness volatile ingredient being directed in Camellia nitidissima active component does not have too much relating to. .
Solid phase micro-extraction technique is proposed by Pawliszyn in nineteen ninety as a kind of novel Sample Pretreatment Technique Used, because it saves solvent and simple to operate quick, is therefore widely used. Stir Bar Sorptive Extraction is a kind of novel SPME Sample Pretreatment Technique, have that stationary phase volume is large, loading capacity is high, without additional stirrer, can avoid competitive adsorption, can when self stirs, realize the advantages such as extracting and enriching, be widely used in the pre-treatment that food, medicine, environmental and biological samples are analyzed. At present, the general direct Stir Bar Sorptive Extraction of solid phase micro-extraction technique: be generally applicable to the extraction of the weak material of non-volatility or volatility, as the weak Tea Polyphenols of volatility in Camellia nitidissima, general flavone, saponins material etc., if directly applying to oiliness volatile ingredient detects, oiliness becomes branch directly to volatilize, and has a strong impact on accordingly the order of accuarcy of detection.
Stir Bar Sorptive Extraction is a kind of technology that is applicable to very much low concentration sample enrichment, the magnetic-adsorption stirring rod that only outer wall need to be wrapped in to sorbing material is put into cup or bottle that sample solution is housed, start many minutes magnetic stirrer a few minutes to ten, the active active ingredient after enrichment will be adsorbed in stirring rod by enrichment. By the enrichment of extraction stirring rod, can there is the ability of multiple concentration lower than the compound of ppb of analyzing.
Stir Bar Sorptive Extraction does not need a large amount of solvent extractions, bioaccumulation efficiency is higher than SPME, because dynamic agitation enrichment, repeatability is also good than SPE, easy to use, is applicable to Camellia nitidissima Active Components, particularly half volatilization or nonvolatile Tea Polyphenols, total flavonoid composition, general stripping trapping technique or headspace analysis technology are difficult to analyze, and still, application solid phase extraction techniques is analyzed said components and had good effect. This technology often realizes the detection of synchronizeing to active ingredient with the coupling such as high performance liquid chromatography, liquid chromatography-mass spectrography, gas chromatography-mass spectrum, Capillary Electrophoresis.
But although stirring rod solid phase extraction techniques is with the obvious advantage, its performance largely depends on the performance of its coating material. the thin layer adsorbed polymer material that traditional stirring rod SPME extracting fiber stirring rod surface used scribbles mostly is perfluorinated resin, polypyrrole, ethylene methacrylic radical siloxane, epoxy-dimethyl silicone polymer etc., these materials are the higher and being fragile of price often, in reality processing, need to ensure absorption property by thickening coating, the thickening of coating can cause and both can reduce detection sensitivity, can improve again the probability that fracture occurs stirring rod coating in actual mechanical process, for example also there will be when active components of plants sample to leave over phenomenon or matrix interference phenomenon at SPE coating material analyzing Cucumber, have a strong impact on the accuracy of detection.
Summary of the invention
The present invention is directed to the problem that prior art exists, the present situation detecting in conjunction with Camellia nitidissima oiliness volatile ingredient, the problem existing for stirring rod SPE detection technique, formed a kind of Camellia nitidissima oils volatile ingredient detection method, have detect accurate, highly sensitive, selective absorption is effective and the feature of long service life.
Content of the present invention is:
A kind of Camellia nitidissima oils volatile ingredient detection method, comprises that SPE absorption-gas chromatography-mass spectrography detects, and described SPE is the extraction of head space stirring rod solid phase adsorption, and described stirring rod scribbles based on two dimension or three-dimensional graphene-polymer coating.
By selecting the coating material of Graphene as stirring rod, can make full use of that excellent mechanical property, quality that Graphene has are light, specific area is large, Young's modulus and the feature such as fracture strength is large, can utilize again its machinery, mechanics, chemistry, electric property excellence, and the advantage that is easy to get of raw material. Therefore, adopt Graphene class nano material to substitute the coating materials such as traditional perfluorinated resin that is applied in stirring rod solid phase extraction techniques, the advantage that the theoretical specific area that can bring into play Graphene is 2630m2/g, effectively increases stirring rod SPE coating super large specific surface. Meanwhile, between graphene-polymer coating material and oiliness volatile ingredient, exist stronger π-π and interact, thereby such material in Camellia nitidissima is had to good selective extraction adsorption effect. Due to graphene-polymer coating machine excellent performance, make above-mentioned material outstanding in High Rotation Speed extraction wearability, young modulus of material and fracture strength are large, can make stirring rod greatly extend service life, thereby are greatly conducive to the reappearance of Camellia nitidissima oiliness volatile ingredient testing result. By adopting head space sorption extraction, can effectively avoid the error that causes at sample feeding, improve the accuracy of SPE, further ensure the accuracy of testing result.
Further, the material of described graphene-polymer coating comprise Graphene and Graphene material modified, described Graphene is material modified comprises graphene oxide, Graphene-polyethylene glycol dimethacrylate, graphene-polypyrrole, Graphene-poly-MTMS and Graphene class nano material.
Further, the material of described graphene-polymer coating is that the activated carbon of preparing with renewable resource carbonization synthesizes by modified Hummers method and reversible addition-fracture chain transfer polymerization method.
Further, described graphene-polymer coating is nano coating. Single-layer graphene often only has 0.7-1.2nm thick, multi-layer graphene-polymer coating also only has several nanometer thickness, materials theory specific area is 2630m2/g, actual specific surface 400-800m2/g, thereby solid phase stirring rod based on Graphene extraction absorbing process can obtain higher extraction quantity, lower detection limit and better reappearance, highly sensitive, wide region and the good reproduction that can realize oiliness volatile ingredient in Camellia nitidissima detect.
Further, the activated carbon that prepared by described renewable resource carbonization raw material comprise straw, bagasse and cornstalk.
Further, described Camellia nitidissima oiliness volatile ingredient comes from blade, fruit, fruit stone, pollen, petal and/or the pistil of Camellia nitidissima.
Further, described oiliness volatile ingredient comprises arbricolin, 1,2-epoxy octadecane, 1,2-Disparmone, irisone, phytol, linoleic acid, methyl linoleate and ethyl linoleate.
Further, described organophosphorous pesticides-mass spectrometry detects as selective and detects.
The invention has the beneficial effects as follows:
The first, detect accurately, by selecting Graphene as stirring rod coating material, adopt selective absorption to replace competitive adsorption, adopt the extraction of head space stirring rod solid phase adsorption to replace and directly stir extraction, effectively improve the order of accuarcy detecting;
The second, highly sensitive, grapheme material is nano level layer material, can enlarge markedly adsorption surface area, reduces the thickness of coating, significantly improves the sensitivity of detection;
Three, selective absorption is effective, and the selective absorption of grapheme material is based on π-pi-conjugated key effect, selectively strong, good separating effect;
Four, long service life, the mechanical performance of grapheme material, mechanical property excellence, abrasive resistance is strong, can extend the service life of stirring rod;
Five, maintenance cost is low, directly carries out selective absorption, reduces the separating step that traditional competitive adsorption is loaded down with trivial details, there is no separation costs, greatly saves the testing cost of routine use and maintenance.
Detailed description of the invention
In order further to understand content of the present invention, be specifically described with regard to summary of the invention and specific embodiment below:
A kind of Camellia nitidissima oils volatile ingredient detection method, comprises that SPE absorption-gas chromatography-mass spectrography detects, and described stirring rod scribbles based on two dimension or three-dimensional graphene-polymer coating. The material of described graphene-polymer coating comprise Graphene and Graphene material modified, described Graphene is material modified comprises graphene oxide, Graphene-polyethylene glycol dimethacrylate, graphene-polypyrrole, Graphene-poly-MTMS and Graphene class nano material. Described graphene-polymer coating is nano coating.
In the concrete preparation of graphene-polymer coating material, can carry out as follows:
The first step, utilize renewable resource carbonization to prepare activated carbon: to select renewable resource to comprise straw, bagasse and cornstalk, take and preferably clean rear dry straw, bagasse or cornstalk, segment is pulverized, cross 30 mesh sieves, put into porcelain crucible, add amount of substance concentration be the liquor zinci chloridi of 0.05mol/L as activator, stir and evenly mix, the feed liquid mixing is at room temperature flooded to 12h. Subsequently the feed liquid of having flooded is put into Muffle furnace, start to rise to 900 DEG C taking heating rate as 10 DEG C/min from room temperature, after insulation certain hour, the sample having activated is taken out from Muffle furnace, immediately sample is poured in certain density aqueous hydrochloric acid solution, then sample is washed with water to pH value is 7. Again the sample having washed is put into electric heating convection oven, dry 4h for 110 DEG C, in drier, leave standstill cooling. Finally sample was pulverized to 300 mesh sieves, obtained straw source activity charcoal crude product. Above-mentioned crude product adopts the Cellu.sep bag filter of specification 6000-8000, dialyses approximately one week at pH in the deionized water that is 7.38, obtains active carbon pure sample after vacuum drying.
Second step, modified Hummers legal system are for graphene oxide: the active carbon that the first step is made sieves, sieve mesh is 300 orders, takes and joins in the mixture of dense H2SO4, K2S2O8 and P2O5, heats above-mentioned mixed system to 80 DEG C, keep this temperature, magnetic agitation 5 hours. Cooling reaction system is to room temperature subsequently, by mixture impouring 500mL deionized water, after hold over night by above-mentioned standing thing through 0.2 micron of membrane filtration, washing is also dried naturally, obtains pre-oxidation graphite. The graphite of this pre-oxidation is joined in the dense H2SO4 of 120ml of 0 DEG C, subsequently, slowly add KMnO4, and control reaction temperature 20 DEG C of stirrings. Potassium permanganate finishes, control reaction system 35 DEG C stir 4 hours, subsequently, add deionized water, and by peripheral ice bath control temperature below 50 DEG C. Stir after 1.5 hours, then add deionized water, after half an hour, dropwise splash into 30% H2O2, reaction system is rapidly by the brown brown color that changes into. Remove agitating device, filter this pale brown mixture, wash to remove metal ion with the HCl that volume ratio is 1:10, use again subsequently deionized water cyclic washing, obtain brown solid, after drying at room temperature, it is 0.5% aqueous dispersions that above-mentioned brown solid is made to mass concentration, dialysis one week, finally filters continuously, washing, again disperse ultrasonic 1 hour, filter, 60 DEG C of vacuum drying 24 hours, can prepare graphene oxide nanometer sheet. Above-mentioned graphene oxide nanometer sheet is scattered in water again, after ultrasonic 30 minutes, adds appropriate hydrazine hydrate, 100 DEG C are refluxed 24 hours, filter, and 60 DEG C of vacuum drying 24 hours, can prepare graphene oxide.
The preparation of the 3rd step, graphene-polymer: activation interpolation pipe. Accurately measure ethylene glycol dimethacrylate, Macrogol 6000, the dimethyl formamide azodiisobutyronitrile of certain mass, ultrasonic vortex is to the solution that obtains clarification. Graphene is added to above-mentioned solution, and making its concentration is 1.0mg/mL, and then in recirculated water, ultrasonic 30min obtains finely dispersed solution, gets in the some 0.6mL of the pouring into centrifuge tubes of above-mentioned pre-polymerization liquid, inserts interpolation pipe, discharges the bubble in solution. After its upper end is sealed with sealing compound and polytetrafluoroethylraw raw material band successively, can in micro-wave oven, react, microwave reaction finishes carefully cated bonding stirring rod to be taken out with Medical forceps afterwards, the methanol/water solution that is 1:1 by volume ratio successively and acetone is coating cleaning on 60 DEG C of shaking tables, and coating is stored in three water for subsequent use after cleaning.
The operating procedure of described extraction is: pluck fresh golden flower prophyll in spring, adopt electronic scale weighing; The fresh golden flower prophyll in spring of plucking is screened, select the freshest and the tenderest, optimum blade, remove second-rate blade; The former leaf raw material of golden flower optimizing must meet the Pharmacopoeia of the People's Republic of China (version in 2010) requirement, without going mouldy, free from extraneous odour, free from admixture; To optimize Camellia nitidissima prophyll clean after, with medicinal herb grinder pulverize, by pulverize after Camellia nitidissima raw material; Get blade, fruit, fruit stone, pollen, petal and/or the pistil of the Camellia nitidissima after a certain amount of pulverizing, cross 120 mesh sieves, the powder after sieving is placed in to head space bottle; Then adopt the stainless steel hook of non-activity Camellia nitidissima powder to be butchered in the stirring rod of porous graphene-polymer coating, stirring rod be placed in bottle apart from bottom approximately 2/3 place, finally with polytetrafluoroethylene (PTFE) rubber cushion bottle cap sealing lid, head space bottle is sealed, at 60 DEG C of temperature, (adopt the heating of bottom electrical heating jacket) and extract 40 minutes.
Detect at the organophosphorous pesticides-mass spectrometry that is applied in the detection of Camellia nitidissima oiliness volatile ingredient, described organophosphorous pesticides-mass spectrometry detects as selective and detects, and described Camellia nitidissima oiliness volatile ingredient comes from blade, fruit, fruit stone, pollen, petal and/or the pistil of Camellia nitidissima. Described oiliness volatile ingredient comprises arbricolin, 1,2-epoxy octadecane, 1,2-Disparmone, irisone, phytol, linoleic acid, methyl linoleate and ethyl linoleate.
After extraction, the stirring rod based on porous graphene-polymer coating having extracted is put in sample sleeve pipe, finally sample sleeve pipe is put into, in AgilentCDS5200 cracker, carry out thermal desorption. Instrument: the instrument U.S. Agilent6890-5973 type gas-chromatography coupling instrument of selecting, setting heating schedule is: be warmed up to 85 DEG C from 25 DEG C of room temperatures with 10 DEG C/min, then be warmed up to 180 DEG C with 10 DEG C/min, be finally warmed up to 250 DEG C with 5 DEG C/min and keep 5 minutes; Set injection port and detector temperature and be 250 DEG C; Split ratio is 30:1; Post flow: 1mL/min, carrier gas is high pure nitrogen; Mass spectrum condition is " high-purity helium, EI ion gun, ionization voltage 70eV; Ion source temperature is 250 DEG C, transmission line temperature: 250 DEG C; Sweep limits: 40-500amu. Finally testing result mass spectrum java standard library Nist spectrogram storehouse is contrasted.
The above, be only preferred embodiment of the present invention, not the present invention done to any pro forma restriction; The those of ordinary skill of all industry all can be implemented the present invention with the above shown in by specification swimmingly; But all those skilled in the art are not departing within the scope of technical solution of the present invention, can utilize disclosed above technology contents and a little change, the modification of making and the equivalent variations developing, be equivalent embodiment of the present invention; Meanwhile, the change of any equivalent variations that all foundations essence technology of the present invention is done above embodiment, modification and differentiation etc., within all still belonging to the protection domain of technical scheme of the present invention.
Claims (6)
1. a Camellia nitidissima oils volatile ingredient detection method, comprise that organophosphorous pesticides-mass spectrometry detects, it is characterized in that: described SPE is the extraction of head space stirring rod solid phase adsorption, and described stirring rod scribbles based on two dimension or three-dimensional graphene-polymer coating;
Described oiliness volatile ingredient comprises arbricolin, 1,2_ epoxy octadecane, 1,2_ Disparmone, irisone, phytol, linoleic acid, methyl linoleate and ethyl linoleate;
Described graphite is rare-and the material of polymer coating is Graphene-polyethylene glycol dimethacrylate.
2. Camellia nitidissima oils volatile ingredient detection method according to claim 1, is characterized in that: the material of described graphene-polymer coating is that the activated carbon of preparing with renewable resource carbonization is synthetic by modified Hummers method and reversible addition-fracture chain transfer polymerization method.
3. Camellia nitidissima oils volatile ingredient detection method according to claim 2, is characterized in that: described graphene-polymer coating is nano coating.
4. Camellia nitidissima oils volatile ingredient detection method according to claim 3, is characterized in that: the raw material of activated carbon prepared by described renewable resource carbonization comprises straw, bagasse and cornstalk.
5. Camellia nitidissima oils volatile ingredient detection method according to claim 4, is characterized in that: described Camellia nitidissima oiliness volatile ingredient comes from blade, fruit, fruit stone, pollen, petal and/or the pistil of Camellia nitidissima.
6. Camellia nitidissima oils volatile ingredient detection method according to claim 5, is characterized in that: described organophosphorous pesticides-mass spectrometry detects as selective and detects.
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| CN110554113B (en) * | 2019-09-12 | 2022-04-01 | 云南中烟工业有限责任公司 | Method for detecting volatile components in tobacco shreds based on SBSE-HS-GC-MS |
| CN110554115B (en) * | 2019-09-20 | 2022-04-01 | 云南中烟工业有限责任公司 | Method for measuring volatile components in tobacco shreds based on SBSE-TD-GC-MS |
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