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
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- 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
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- Prior art keywords
- propane
- oil
- standard
- gas
- sample
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- 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
- Sampling And Sample Adjustment (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (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.
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CN201210545709.0A CN103033574B (en) | 2012-12-17 | 2012-12-17 | Method for detecting residual solvent in subcritical propane extraction product |
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CN201210545709.0A CN103033574B (en) | 2012-12-17 | 2012-12-17 | Method for detecting residual solvent in subcritical propane extraction product |
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CN103033574A CN103033574A (en) | 2013-04-10 |
CN103033574B true CN103033574B (en) | 2014-12-24 |
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CN201210545709.0A Expired - Fee Related CN103033574B (en) | 2012-12-17 | 2012-12-17 | Method for detecting residual solvent in subcritical propane extraction product |
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Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
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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 |
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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 |
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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 |
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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 |
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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 |