CN103033574B - Method for detecting residual solvent in subcritical propane extraction product - Google Patents
Method for detecting residual solvent in subcritical propane extraction product Download PDFInfo
- Publication number
- CN103033574B CN103033574B CN201210545709.0A CN201210545709A CN103033574B CN 103033574 B CN103033574 B CN 103033574B CN 201210545709 A CN201210545709 A CN 201210545709A CN 103033574 B CN103033574 B CN 103033574B
- Authority
- CN
- China
- Prior art keywords
- propane
- oil
- standard
- gas
- sample
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 226
- 239000001294 propane Substances 0.000 title claims abstract description 112
- 238000000605 extraction Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000013557 residual solvent Substances 0.000 title claims 2
- 239000000243 solution Substances 0.000 claims abstract description 16
- 238000001514 detection method Methods 0.000 claims abstract description 13
- 238000012360 testing method Methods 0.000 claims abstract description 12
- 239000011550 stock solution Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000012530 fluid Substances 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract 2
- 239000007789 gas Substances 0.000 claims description 30
- 238000003988 headspace gas chromatography Methods 0.000 claims description 15
- 239000012086 standard solution Substances 0.000 claims description 12
- 238000004817 gas chromatography Methods 0.000 claims description 7
- 238000004458 analytical method Methods 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 238000011084 recovery Methods 0.000 claims description 4
- 238000009834 vaporization Methods 0.000 claims description 4
- 230000008016 vaporization Effects 0.000 claims description 4
- 238000005259 measurement Methods 0.000 claims description 3
- 238000011156 evaluation Methods 0.000 claims description 2
- 238000002309 gasification Methods 0.000 claims description 2
- 150000002431 hydrogen Chemical class 0.000 claims description 2
- 238000010606 normalization Methods 0.000 claims description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 4
- 235000013305 food Nutrition 0.000 abstract description 4
- 238000007689 inspection Methods 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 52
- 235000019198 oils Nutrition 0.000 description 52
- 239000004519 grease Substances 0.000 description 11
- 229910000831 Steel Inorganic materials 0.000 description 9
- 239000010959 steel Substances 0.000 description 9
- 239000011159 matrix material Substances 0.000 description 8
- 244000068988 Glycine max Species 0.000 description 6
- 235000010469 Glycine max Nutrition 0.000 description 6
- 210000001161 mammalian embryo Anatomy 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 4
- 235000019774 Rice Bran oil Nutrition 0.000 description 4
- 239000001273 butane Substances 0.000 description 4
- 239000000284 extract Substances 0.000 description 4
- 239000003915 liquefied petroleum gas Substances 0.000 description 4
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 4
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 4
- 239000008165 rice bran oil Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000007865 diluting Methods 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012417 linear regression Methods 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 229930014626 natural product Natural products 0.000 description 3
- 238000009423 ventilation Methods 0.000 description 3
- 239000010497 wheat germ oil Substances 0.000 description 3
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 239000006057 Non-nutritive feed additive Substances 0.000 description 1
- 229910018503 SF6 Inorganic materials 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000001282 iso-butane Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 230000005180 public health Effects 0.000 description 1
- 238000012372 quality testing Methods 0.000 description 1
- 230000010076 replication Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 1
- 229960000909 sulfur hexafluoride Drugs 0.000 description 1
- 239000006200 vaporizer Substances 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
本发明涉及亚临界丙烷萃取产品中溶剂残留的检测方法，涉及食品安全检测领域。是先将丙烷标准气通入与待测油相同油种但不含丙烷的成品油中，充分稳定，准确称量，得到该储备液的浓度，然后将其稀释配制一系列丙烷标准油溶液，取该系列标准油溶液5.00～100.00g置于135mL顶空瓶中，在40～70℃恒温水浴条件下以500rpm的转速搅拌平衡10～60min，用微量进样器取其上层气体进行顶空气相色谱分析，相同条件下测待测油样品中残留丙烷峰面积，根据标准曲线，即可求得油样品中残留丙烷含量。该方法成本低、操作简便以及专属性强等优点，可广泛应用于油脂的亚临界流体加工企业及粮油检测机构的粮油品质检验与控制。
The invention relates to a detection method for solvent residues in subcritical propane extraction products, and relates to the field of food safety detection. The method is to inject the propane standard gas into the refined oil of the same type as the oil to be tested but without propane, fully stabilize and accurately weigh to obtain the concentration of the stock solution, and then dilute it to prepare a series of propane standard oil solutions. Take 5.00～100.00g of this series of standard oil solutions and place them in a 135mL headspace bottle, stir and balance at a speed of 500rpm in a constant temperature water bath at 40～70℃ for 10～60min, and use a micro sampler to take the upper layer gas for headspace phase For chromatographic analysis, the residual propane peak area in the oil sample to be tested is measured under the same conditions, and the residual propane content in the oil sample can be obtained according to the standard curve. The method has the advantages of low cost, simple operation and strong specificity, and can be widely used in the inspection and control of grain and oil quality in oil subcritical fluid processing enterprises and grain and oil testing institutions.
Description
Technical field
The present invention relates to field of detection of food safety, refer in particular to a kind of method adopting gas chromatography to detect dissolvent residual in the edible oil and fat product of Propane fluid extraction fast, the method can be grease production enterprise and Safety of Food Quality testing agency supplying method foundation.
Background technology
Subcritical fluids refers to that some compound is higher than its boiling point but lower than under the condition of critical temperature and emergent pressure, the material existed with fluid form.Subcritical fluid extraction technology is then for solvent with subcritical fluids or its mixed solution, a kind of new technology of target components is extracted from natural products, be particularly suitable for the extraction of volatile oil in natural products, grease or liposoluble constituent, the change technology there is normal temperature leaching, low temperature desolventizing, do not destroy the outstanding advantage of heat-sensitive ingredients, be an environmental protection, having a extensive future.
The subcritical fluids being usually used in valuable grease production or effective components from natural materials extraction comprises: propane, butane, liquefied petroleum gas (LPG) (LPG), high-purity isobutane (R600a), 1,1,1,2-HFC-134a (R134a), dimethyl ether (DME) and sulfur hexafluoride etc., be wherein most widely used with propane, butane, LPG.The Ministry of Public Health of China includes propane in food processing aid catalogue in 2008, but has hypotoxicity due to it to nerve system of human body, so, be a food-safety problem that can not be ignored with dissolvent residual in the product of Propane extraction.
At present, Propane extraction grease in propane residue detection there is no unified national standard.Due to not enough to its attention degree, so far the research of the detection method about propane in grease is not had, and mensuration being most widely used with headspace gas chromatography of dissolvent residual in the vegetable oil products of conventional solvent extraction, GB5009.37-2003 just adopts this method to detect the residual quantity of No. six solvents.But because be gaseous state under propane normal temperature and pressure, and normal hexane is in a liquid state, and in contrast, it can not dissolve each other preferably with grease, makes the standard oil solution accurately cannot preparing propane, thus hinders the quantitative detection of residual propane in grease.
The people such as Xu Yun report the method with the propane in infrared spectrophotometer and Headspace-Gas Chromatography Analysis wastewater measurement, butane.Although this method determines the content of propane in waste water, butane.But researchist is not mixed with standard items by soluble in water for propane, but directly with the Standard Gases sample introduction of variable concentrations, the matrix of standard items and testing sample is inconsistent, causes the inaccurate of measurement, matrix simultaneously containing propane compared with grease is different, because the method is inadvisable.
For this reason, two key technical problems must be solved: first when adopting headspace gas chromatography to detect dissolvent residual in Propane extracted products, when preparation standard solution, propane can dissolve each other well with matrix oil, accurately could obtain variable concentrations (series) propane solution; Secondly, the matrix of standard solution must be consistent with the matrix of testing sample, and like this, the concentration that both balance rear headspace gas just has comparability.
In order to solve above-mentioned two key technical problems, propane calibrating gas first passes in the matrix oil (not containing propane) same with oil phase to be measured by the present invention, make it be fully absorbed, then above-mentioned propane solution is carried out uncovered be placed to stable, diluted again, thus preparation obtains a series of propane standard oil solution.
Summary of the invention
The present invention solves the technical scheme that its detection technique adopts: take not containing the product oil of propane, propane is passed in this product oil, stop after a period of time passing into propane gas, weigh the quality of product oil after a period of stabilisation, obtain the concentration of propane in this oil; Then a certain amount of above-mentioned propane solution product oil is diluted, to prepare the propane oil solution of a series of concentration, under being placed in ml headspace bottle uniform temperature, balance a period of time, get head space gases in bottle and carry out head space gas chromatography, record peak area, drawing standard curve; Again by the testing sample of identical amount, under the same conditions, carry out head space gas chromatography, record peak area, contrasts above-mentioned typical curve, obtains the content of propane in head space gases; Finally be converted to the content of propane in testing sample.
Above-mentioned purpose of the present invention is realized by following steps: the detection method of dissolvent residual in Propane fluid extraction product, carries out according to following step:
(1) preparation of standard reserving solution:take not containing the product oil quality m of propane
1(20.0000 ~ 200.0000 g), propane gas is passed into 10 ~ 60 min in this oil, wherein preferred 20 ~ 40 min, and rear stopping passes into propane gas, then ambient-temp-stable 12 ~ 96 h, and wherein preferably after 48 ~ 84 h, the quality again weighing oil is m
2, the weight of increase is the quality passing into propane gas, obtains the concentration of propane in oil:
X
1=1000(m
2－m
1)/?m
1
In formula:
X
1--the concentration of propane in oil, unit is milligram every gram (mg/g);
M
1--not containing the quality of propane product oil, unit is gram (g);
M
2--quality oily after passing into propane, unit is gram (g).
(2) preparation of series standard solution:pipette storing solution stable in the step (1) that quality is m ' in the tool plug ml headspace bottle of clean drying, close plug, obtains the quality of propane in product oil (mg): m ' × X
1, in this bottle, add the product oil not containing propane is m(5.00 ~ 50.00g to oily quality), close plug, mixed preparing obtains the titer of a series of different propane concentration, and concentration is (m ' × X
1)/m
In formula:
M '--pipette the amount of propane standard reserving solution, unit is gram (g);
M--is used for the oil sample amount of gas chromatographic detection, and unit is gram (g).
(3) head space gas chromatography:by the fat solution of the different propane concentrations of (m) identical in quality in step (2), balance 10 ~ 60 min is stirred with the rotating speed of 500 rpm in 40 ~ 70 DEG C of thermostat water baths, insertion microsyringe or syringe pipette gasification bottle top tank air 100 μ L immediately, carry out head space gas chromatography, write down peak area, take peak area as ordinate, propane concentration is horizontal ordinate, drawing standard curve; Wherein GC conditions is: preferred column HP-PLOT Al
2o
3-S(15m*0.53 mm*15.00 μm), flame ionization ditector (FID), column temperature 40 ~ 100 DEG C, the temperature of vaporizer and detecting device 150 ~ 250 DEG C, carrier gas (N
2) 7.2 mL/min, hydrogen 50 mL/min, air 500 mL/min, the testing sample pipetting (m) identical in quality is deposited in the tool plug ml headspace bottle of volume same as described above, close plug, under the same conditions, carries out head space gas chromatography, write down the peak area (multiple chromatographic peak normalization method) that component is measured, contrast standard opisometer calculates propane content in testing sample (mg/kg): X=1000X
2
In formula:
X
2--the content of propane in testing sample, unit is milligram every gram (mg/g);
The content of propane in X--testing sample, unit is milligrams per kilogram (mg/kg).
(4) evaluation of method accuracy:by head space equilibrium condition and the GC conditions of step (3), 6 parallel replications are carried out to testing sample (oil and fat product of propane extraction), calculates dissolvent residual in sample according to typical curve, and calculate relative standard deviation (RSD)≤5.5%; Again this sample is carried out recovery of standard addition test, add the standard items (high, normal, basic concentration) of three levels, average recovery of standard addition is 95 ~ 110%, RSD is 1 ~ 5.5%.
The product oil not containing propane of the present invention refers to that same oil plant or natural products adopt No. 6 solvents, sherwood oil, supercritical COs
2or the grease that the extraction such as milling process obtains, or the product oil that Propane extracts is carried out 100 DEG C of heating 12 ~ 24 h, drain propane wherein.
Advantage of the present invention:
(1) the present invention gives sufficient inflationtime and suitable stable standing time to the product oil not containing propane and weighs accurately, product oil is absorbed well to propane calibrating gas dissolve each other and reach certain balance, overcoming propane calibrating gas is injected directly in grease, the deficiency of its dissolubility and poor stability, improves the accuracy of propane residue detection;
(2) the present invention adopts the oil same with oil phase to be measured to be matrix oil, propane is identical with the Interaction Force of oil to be measured with matrix oil, there is identical adsorption-desorption mobile equilibrium, therefore when headspace gas chromatography sample introduction, the final equilibrium system of propane oil solution does not change, and the experimental data recorded is accurate;
(3) content that the present invention adopts headspace gas chromatography to detect propane in valuable grease has that cost is low, easy and simple to handle, specificity is strong and pollute the advantages such as little to instrument system.
Accompanying drawing explanation
Fig. 1 is that in example 1, concentration is the propane soybean embryo fat/oil standard solution gas chromatogram of 0.0021 mg/g,
The soybean embryo fat/oil product gas chromatogram of propane extraction to be measured in Fig. 2 example 1,
Propane typical curve obtained in Fig. 3 example 1.
Embodiment
Below in conjunction with embodiment, the present invention is further elaborated.
embodiment 1
Get commercially available No. 6 solvent-extracted soybean embryo fat/oil 50.0000 g, the 150ml loading homemade clean dried constant weight ventilates in bottle (comprising plastic bottle with cover, draft tube and gas outlet).Propane calibrating gas is stored in steel cylinder, the valve controlling flow is had above steel cylinder, communicate with the external world with rubber tube, separately get one section of rubber tube to be communicated with the rubber tube of steel cylinder by emulsion tube, gross mass 110.3620 g of oil and air-breather, open cylinder valve, propane calibrating gas is slowly passed in product oil, valve-off after 0.5 h, the gross mass weighing oil solution and air-breather is 111.3323 g, standing at room temperature places 72h, again weigh the gross mass of product oil and air-breather, its steady quality does not change in 110.3624(1h), the quality relatively increased before and after ventilation is the quality of fat absorption propane, thus obtain the Standard Stock solutions that concentration is 0.0080mg/g, get the Standard Stock solutions of certain mass and soybean embryo fat/oil mixed diluting quantitatively to 10.00 g not containing propane, obtained propane concentration of standard solution is followed successively by 0.0041 mg/g, 0.00031 mg/g, 0.0021 mg/g, 0.0010 mg/g, 0.0008 mg/g, 0.0004 mg/g, 0.0002 mg/g, and by its series standard solution close plug in 135 mL ml headspace bottle, balance 15 min is stirred with the rotating speed of 500 rpm respectively in 50 DEG C of thermostat water baths, from ml headspace bottle, 100 μ L top tank airs are extracted immediately with microsyringe, pass through gas chromatographic analysis, write down component peaks area, with peak area, linear regression is carried out to propane concentration, obtaining regression equation is y=565377x-57.101, correlation coefficient r=0.9991, the range of linearity is 0.0002 ~ 0.0041 mg/g.Get the soybean germ oil product (laboratory obtains) of 10.00 g Propane extractions, close plug in 135 mL ml headspace bottle, water bath with thermostatic control 15 min at 50 DEG C, from bottle, extract 100 μ L with micro syringe immediately and carry out analysis headspace gas chromatography, write down each component peaks area, comparison typical curve, the residual quantity calculating propane in the soybean embryo fat/oil of Propane extraction is 0.22mg/kg.
Wherein gas chromatography reference conditions:
Chromatographic column: HP-PLOT Al
2o
3-S (15m*0.53mm*15.00 μm)
Detecting device: FID
Column temperature: 70 DEG C
Temperature of vaporization chamber: 180 DEG C
Detector temperature: 210 DEG C
Carrier gas (N
2): 7.2 mL/min
Hydrogen: 50 mL/min
Air: 500 mL/min
embodiment 2
Get supercritical CO
2wheat-germ oil 100.0000 g of extraction, the 150ml loading homemade clean dried constant weight ventilates in bottle.Propane calibrating gas is stored in steel cylinder, the valve controlling flow is had above steel cylinder, communicate with the external world with rubber tube, separately get one section of rubber tube to be communicated with the rubber tube of steel cylinder by emulsion tube, gross mass 160.3453 g of oil and air-breather, open cylinder valve, propane calibrating gas is slowly passed in product oil, valve-off after 1 h, the gross mass weighing oil and air-breather is 161.9173 g, standing at room temperature places 84h, again weigh the gross mass of product oil and air-breather, its steady quality does not change in 160.3467(1h), the quality relatively increased before and after ventilation is the quality of fat absorption propane, thus obtain the Standard Stock solutions that concentration is 0.0140mg/g, get the Standard Stock solutions of certain mass and wheat-germ oil mixed diluting quantitatively to 10.00 g not containing propane, obtained propane concentration of standard solution is followed successively by 0.0070 mg/g, 0.0053 mg/g, 0.0035 mg/g, 0.0028 mg/g, 0.0014 mg/g, 0.0006 mg/g, 0.0003 mg/g, 0.0001 mg/g, and by its series standard solution close plug in 135 mL ml headspace bottle, balance 15 min is stirred with the rotating speed of 500 rpm respectively in 50 DEG C of thermostat water baths, from ml headspace bottle, 100 μ L top tank airs are extracted immediately with microsyringe, pass through gas chromatographic analysis, write down peak area, with peak area, linear regression is carried out to propane concentration, obtaining regression equation is y=507627x-36.541, correlation coefficient r=0.9997, the range of linearity is 0.0001 ~ 0.0070 mg/g.Get the wheat embryo oil product (commercially available) of 10.00 g Propane extractions, close plug in 135 mL ml headspace bottle, at 50 DEG C of water bath with thermostatic control 15 min, from bottle, extract 100 μ L with micro syringe immediately and carry out analysis headspace gas chromatography, write down component peaks area, the above-mentioned typical curve of comparison, calculates solvent residual amount in the wheat-germ oil of Propane extraction and does not detect.
Wherein gas chromatography reference conditions:
Chromatographic column: HP-PLOT Al
2o
3-S (15m*0.53mm*15.00 μm)
Detecting device: FID
Column temperature: 40 DEG C
Temperature of vaporization chamber: 150 DEG C
Detector temperature: 250 DEG C
Carrier gas (N
2): 7.2 mL/min
Hydrogen: 50 mL/min
Air: 500 mL/min
embodiment 3
Get commercially available No. 6 solvent-extracted rice bran oil 50.0000 g, the 150ml loading homemade clean dried constant weight ventilates in bottle (comprising plastic bottle with cover, draft tube and gas outlet).Propane calibrating gas is stored in steel cylinder, the valve controlling flow is had above steel cylinder, communicate with the external world with rubber tube, separately get one section of rubber tube to be communicated with the rubber tube of steel cylinder by emulsion tube, gross mass 110.3620 g of oil and air-breather, open cylinder valve, propane calibrating gas is slowly passed in product oil, valve-off after 0.5 h, the gross mass weighing oil solution and air-breather is 111.3329 g, static placement 72 h of difference under room temperature, again weigh the gross mass of product oil and air-breather, its steady quality does not change in 110.3625(1h), the quality relatively increased before and after ventilation is the quality of fat absorption propane, thus obtain the Standard Stock solutions that concentration is 0.0100mg/g, the Standard Stock solutions getting certain mass respectively with rice bran oil mixed diluting quantitatively to 10.00 g not containing propane, obtained propane concentration of standard solution is followed successively by 0.0050 mg/g, 0.00038 mg/g, 0.0025 mg/g, 0.0020 mg/g, 0.0010 mg/g, 0.0005 mg/g, 0.0003 mg/g, and by its series standard solution close plug in 135 mL ml headspace bottle, balance 15 min is stirred with the rotating speed of 500 rpm respectively in 50 DEG C of thermostat water baths, from ml headspace bottle, 100 μ L top tank airs are extracted immediately with microsyringe, pass through gas chromatographic analysis, write down component and record peak area, with peak area, linear regression is carried out to propane concentration, obtaining regression equation is y=565468x-168.261, correlation coefficient r=0.9991, the range of linearity is 0.0003 ~ 0.0050 mg/g.Get the rice bran oil product (laboratory obtains) of 10.00 g Propane extractions, close plug in 135 mL ml headspace bottle, water bath with thermostatic control 15 min at 50 DEG C, from bottle, extract 100 μ L top tank airs with micro syringe immediately and carry out analysis headspace gas chromatography, write down component peaks area, the above-mentioned typical curve of comparison, calculates solvent residual amount in the rice bran oil of Propane extraction and does not detect.
Wherein gas chromatography reference conditions:
Chromatographic column: HP-PLOT Al
2o
3-S (15m*0.53mm*15.00 μm)
Detecting device: FID
Column temperature: 70 DEG C
Temperature of vaporization chamber: 180 DEG C
Detector temperature: 210 DEG C
Carrier gas (N
2): 7.2 mL/min
Hydrogen: 50 mL/min
Air: 500 mL/min.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210545709.0A CN103033574B (en) | 2012-12-17 | 2012-12-17 | Method for detecting residual solvent in subcritical propane extraction product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210545709.0A CN103033574B (en) | 2012-12-17 | 2012-12-17 | Method for detecting residual solvent in subcritical propane extraction product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103033574A CN103033574A (en) | 2013-04-10 |
| CN103033574B true CN103033574B (en) | 2014-12-24 |
Family
ID=48020687
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210545709.0A Expired - Fee Related CN103033574B (en) | 2012-12-17 | 2012-12-17 | Method for detecting residual solvent in subcritical propane extraction product |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103033574B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103743829A (en) * | 2013-11-29 | 2014-04-23 | 山东省化工研究院 | Method for detecting purity of propane and hydrocarbon impurities in propane |
| CN108303479A (en) * | 2018-01-24 | 2018-07-20 | 吉林省百利生物科技有限公司 | The assay method of solvent residual amount in a kind of edible vegetable oil |
| CN109374804B (en) * | 2018-10-31 | 2020-11-03 | 内蒙古中煤蒙大新能源化工有限公司 | Chromatographic analysis method for propane product in methanol-to-olefin process production |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101858893A (en) * | 2009-04-07 | 2010-10-13 | 北京协和药厂 | Headspace gas chromatography detection method of residual solvents in macroporous resin extract |
| CN102288686A (en) * | 2010-06-17 | 2011-12-21 | 河北以岭医药研究院有限公司 | Method for measuring residual amount of organic solvent in traditional Chinese medicine freeze-drying injection |
| CN102323353A (en) * | 2011-08-16 | 2012-01-18 | 上海新先锋药业有限公司 | Method for detecting organic solvent residues in liposome medicines |
-
2012
- 2012-12-17 CN CN201210545709.0A patent/CN103033574B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN103033574A (en) | 2013-04-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112595786B (en) | Quantitative detection method for volatile flavor substances in fermented grains | |
| CN101852783B (en) | Headspace solid-phase microextraction-gas chromatography-mass spectrometry method for detecting hogwash oil | |
| Descamps et al. | Solubility of hydrogen in methanol at temperatures from 248.41 to 308.20 K | |
| CN103033574B (en) | Method for detecting residual solvent in subcritical propane extraction product | |
| Ma et al. | Determination of ethyl carbamate in wine by matrix modification-assisted headspace single-drop microextraction and gas chromatography–mass spectrometry technique | |
| CN102680596B (en) | Method for detecting organic volatile matters in adhesive for cigarettes | |
| CN105954380A (en) | Determination method for linarin in Buddleja officinalis | |
| Hu et al. | A novel method to quantify the activity of alcohol acetyltransferase Using a SnO2-based sensor of electronic nose | |
| Ke et al. | Comparison of fully-automated headspace single drop microextraction and headspace solid phase microextraction techniques for rapid analysis of No. 6 solvent residues in edible oil | |
| CN110412174A (en) | Head space droplet extraction-chromatographic detection method of residual solvent in a kind of grease | |
| Mielle et al. | An alternative way to improve the sensitivity of electronic olfactometers | |
| Liu et al. | A novel method for the determination of the ethanol content in soy sauce by full evaporation headspace gas chromatography | |
| Jin et al. | Determination and calculation of solubility of bisphenol A in supercritical carbon dioxide | |
| Baba-Ahmed et al. | New equipment using a static analytic method for the study of vapour–liquid equilibria at temperatures down to 77 K | |
| CN109781896B (en) | A standard series and gas sample analysis method based on internal standard method | |
| CN103018369B (en) | Detecting method for solvent residues in liquefied petroleum gas extraction products | |
| CN106018631A (en) | Analysis method for solvent residue of extract additive | |
| CN101581707A (en) | Method for simultaneously detecting acetylmethylcar-binol and ligustrazine in table vinegar | |
| Subramoney et al. | Experimental (vapour+ liquid) equilibrium data and modelling for binary mixtures of decafluorobutane with propane and 1-butene | |
| CN106018625A (en) | Method for detecting eucalyptol in moxa sticks | |
| CN105467030A (en) | Method for detecting benzene series in dairy product | |
| CN103033576B (en) | The detection method of dissolvent residual in subcritical butane extracted products | |
| Ndocko Ndocko et al. | Process design method for manufacturing of natural compounds and related molecules | |
| Sidisky et al. | Mixing water and gas: the quantitative measurement of water by gas chromatography using ionic liquid capillary columns | |
| CN104215720A (en) | Method for determining specific transfer volume of low-molecule aldehyde ketone in paper and paperboards |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| CB03 | Change of inventor or designer information |
Inventor after: Xu Bin Inventor after: Jiang Song Inventor after: Zhou Shilong Inventor after: Dong Ying Inventor after: Sun Jun Inventor after: Qi Kun Inventor after: Zhu Xinliang Inventor before: Xu Bin Inventor before: Jiang Song Inventor before: Zhou Shilong Inventor before: Dong Ying Inventor before: Sun Jun |
|
| COR | Change of bibliographic data | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20160415 Address after: 455113, Henan, Anyang hi tech Zone, Henan Province, Chung song street, southern section of Hong 200 meters Patentee after: Henan Yalinjie Biological Technology Co., Ltd. Address before: Zhenjiang City, Jiangsu Province, 212013 Jingkou District Road No. 301 Patentee before: Jiangsu University |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20141224 Termination date: 20181217 |