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CN104387307B - The minimizing technology of ethoxyquinoline in a kind of lutein extract - Google Patents

The minimizing technology of ethoxyquinoline in a kind of lutein extract Download PDF

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Publication number
CN104387307B
CN104387307B CN201410656647.XA CN201410656647A CN104387307B CN 104387307 B CN104387307 B CN 104387307B CN 201410656647 A CN201410656647 A CN 201410656647A CN 104387307 B CN104387307 B CN 104387307B
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ethoxyquinoline
normal hexane
solution
lutein extract
layer
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CN104387307A (en
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黄利勇
李俊和
贾五江
韩文杰
李凤飞
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Chenguang biotechnology group Tengchong Co., Ltd
Chenguang Biotech Group Co Ltd
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Chenguang Biotech Group Co Ltd
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Abstract

The present invention relates to the minimizing technology of ethoxyquinoline in a kind of lutein extract, belong to plant milk extract technical field, comprise the following steps: (1) marigold flower particle, through normal hexane extraction, filtration, concentrating under reduced pressure, obtains xenthophylls extracting solution; (2) in xenthophylls extracting solution, add alcohol solution, stir in 35-55 DEG C of water bath with thermostatic control and obtain mixed solution; (3) layering: mixed solution, at temperature 35-55 DEG C, through centrifugal layering or stratification, is released lower floor's alcoholic solution layer, obtained upper strata normal hexane layer; (4) wash: normal hexane layer clear water washing in upper strata is neutral to water layer pH; (5) concentrated: normal hexane layer concentrates and namely obtains not containing the lutein extract of ethoxyquinoline.The inventive method is simple to operate, and without the need to special equipment, special chemical reagent, treatment capacity is large, and product yield is high, can obtain not containing the lutein extract of ethoxyquinoline, and realize suitability for industrialized production.

Description

The minimizing technology of ethoxyquinoline in a kind of lutein extract
Technical field
The invention belongs to plant milk extract technical field, be specifically related to the minimizing technology of ethoxyquinoline in a kind of lutein extract.
Background technology
Fresh Flos Tagetis Erectae is through gathering-enzymolysis-dehydration-oven dry-granulation-leaching-lutein extract.Lutein extract can obtain the serial xenthophylls products such as lutein crystal, lutein ester, Xanthin micro-capsule through further deep processing.
Ethoxyquinoline, chemical name is 6-oxyethyl group-2,2,4-trimethylammonium-1,2-dihydroquinoline, is one of feed antioxidant of excellent property, and has certain mildew-resistant and freshening effect; Separately can be used as food antioxidant, fruit antistaling agent, rubber antioxidant, be widely adopted in the world at present.
Along with the continuous progress of society and the raising day by day of living standards of the people, while day by day the increasing of xenthophylls market demand, the requirement of people to Product Safety is more and more higher.Found by long-term research, in the xenthophylls product of domestic and international production, some can detect the ethoxyquinoline of trace or trace, present stage, mechanism was still not clear, and potential food safety risk is also uncertain, but under the severe situation of food safety, be necessary to develop a kind of method removing ethoxyquinoline.
Publication number is in the patent of CN101486671, adds sorbent material in Flower of Aztec Marigold extracting solution, stirs after 0.5 ~ 5 hour and filter at 20 ~ 70 DEG C, obtains not containing the product of ethoxyquinoline after mother liquor concentrations.Because adsorbent amount is large, and direct extracting solution does and adsorbs, and there will be product yield low, the shortcoming that treatment capacity is little, is difficult to suitability for industrialized production.
Summary of the invention
In order to overcome the shortcoming of prior art, the invention provides the minimizing technology of ethoxyquinoline in a kind of lutein extract, the method treatment capacity is large, and yield is high, the ethoxyquinoline in lutein extract can be removed to below 5ppb.
The object of the present invention is to provide the minimizing technology of ethoxyquinoline in a kind of lutein extract, comprise the following steps:
(1) marigold flower particle is through normal hexane extraction, filtration, concentrating under reduced pressure, obtains xenthophylls extracting solution;
(2) in xenthophylls extracting solution, add alcohol solution, stir in 35-55 DEG C of water bath with thermostatic control and obtain mixed solution;
(3) layering: mixed solution, at temperature 35-55 DEG C, through centrifugal layering or stratification, is released lower floor's alcoholic solution layer, obtained upper strata normal hexane layer;
(4) wash: normal hexane layer clear water washing in upper strata is neutral to water layer pH;
(5) concentrated: normal hexane layer concentrates and namely obtains not containing the lutein extract of ethoxyquinoline.
In the present invention, the pH value of the alcohol solution added in described step (2) is 2-4, and preferably, described pH value is 2-3.
In the present invention, the alcohol solution added in described step (2) is volume fraction is 30-60% methyl alcohol or aqueous ethanolic solution, and preferably, described alcohol solution is volume fraction is 45-50% methyl alcohol or aqueous ethanolic solution.
In the present invention, be evaporated in described step (1) that lutein extract weight accounts for extracting liquid volume 30% ~ 70%.
In the present invention, the alcohol solution phosphoric acid in described step (2), hydrochloric acid, citric acid adjust ph.
In the present invention, in described step (2), the volume ratio of extracting solution and alcohol solution is 1:1-4.
In the present invention, the water bath with thermostatic control in described step (2) is 35-55 DEG C, and stir 30-60min, preferably described water bath with thermostatic control is 40-45 DEG C.
In the present invention, the normal hexane layer obtained in described step (3) repeats 3-6 time according to step (2), (3) again.
Ethoxyquinoline detection method reference " high performance liquid chromatography-tandem mass method measures ethoxyquinoline in fruit and remains " in the present invention, Ding Tao etc., mass spectrum journal, the 30th volume the 5th phase, 307-310 page, in September, 2009.Present method detects and is limited to 5ppb.
Mentality of designing of the present invention is: ethoxyquinoline solubleness in alcohol solution is comparatively large, and by regulating pH, heating up to increase its solubleness in alcohol solution, and then competes out from normal hexane by it.And lutein extract is almost insoluble in alcohol solution, product yield is high.
Beneficial effect of the present invention is: this technological operation is simple, and without the need to special equipment, special chemical reagent, treatment capacity is large, and product yield is high, can obtain not containing the lutein extract of ethoxyquinoline, and realize suitability for industrialized production.
Embodiment
Below in conjunction with embodiment, the present invention is further detailed explanation.
Embodiment 1
(1), 1000kg marigold flower particle through normal hexane extraction, filtration, concentrated after, obtain 200 liters of xenthophylls extracting solutions, detecting medicinal extract content through sampling is 50%, and total lutein content is 12000g, and in lutein extract, ethoxyquinoline content is 300ppb;
(2), in xenthophylls extracting solution, add the methanol solution (methanol solution phosphoric acid adjust pH to 2.5) of 400 liters of volume fractions 45%, stir 35 minutes in 40 DEG C, obtain mixed solution;
(3), mixed solution in the separator temperature 40 DEG C insulation leave standstill 1 hour, mixed solution is layered as normal hexane layer and methanol layer, is released by methanol layer;
(4), normal hexane layer washes 4 times by step (2), (3);
(5), upper strata normal hexane layer clear water washs to pH=7;
(6), normal hexane layer is concentrated obtains xenthophylls 100kg, total lutein content 11940g, content yield 99.50%; Use high performance liquid phase to detect ethoxyquinoline, do not detect (present method detects and is limited to 5ppb).
Embodiment 2
(1), 1500kg marigold flower particle through normal hexane extraction, filtration, concentrated after, obtain 250 liters of xenthophylls extracting solutions, detecting medicinal extract content through sampling is 45%, and total lutein content is 13400g, and in lutein extract, ethoxyquinoline content is 500ppb;
(2), in xenthophylls extracting solution, add the ethanolic soln (ethanolic soln hydrochloric acid adjust pH to 2.2) of 750 liters of volume fractions 48%, stir 50 minutes in 45 DEG C, obtain mixed solution;
(3), mixed solution in the separator temperature 45 C insulation leave standstill 1.5 hours, mixed solution is layered as normal hexane layer and alcohol layer, is released by alcohol layer;
(4), normal hexane layer washes 5 times by step (2), (3);
(5), upper strata normal hexane layer clear water washs to pH=7;
(6), normal hexane layer is concentrated obtains xenthophylls 112.5kg, total lutein content 13250g, content yield 98.88%; Use high performance liquid phase to detect ethoxyquinoline, do not detect.
Embodiment 3
(1), 1000kg marigold flower particle through normal hexane extraction, filtration, concentrated after, obtain 750 liters of xenthophylls extracting solutions, detecting medicinal extract content through sampling is 30%, and total lutein content is 12000g, and in lutein extract, ethoxyquinoline content is 700ppb;
(2), in xenthophylls extracting solution, add the methanol solution (methanol solution phosphoric acid adjust pH to 4.0) of 750 liters of volume fractions 60%, stir 30 minutes in 35 DEG C, obtain mixed solution;
(3), mixed solution in the separator temperature 35 DEG C insulation leave standstill 1 hour, mixed solution is layered as normal hexane layer and methanol layer, is released by methanol layer;
(4), normal hexane layer washes 6 times by step (2), (3);
(5), upper strata normal hexane layer clear water washs to pH=7;
(6), normal hexane layer is concentrated obtains xenthophylls 100kg, total lutein content 11921g, content yield 99.34%; Use high performance liquid phase to detect ethoxyquinoline, do not detect.
Embodiment 4
(1), 1500kg marigold flower particle through normal hexane extraction, filtration, concentrated after, obtain 200 liters of xenthophylls extracting solutions, detecting medicinal extract content through sampling is 70%, and total lutein content is 13500g, and in lutein extract, ethoxyquinoline content is 400ppb;
(2), in xenthophylls extracting solution, add the ethanolic soln (ethanolic soln hydrochloric acid adjust pH to 3.0) of 800 liters of volume fractions 50%, stir 60 minutes in 55 DEG C, obtain mixed solution;
(3), mixed solution in the separator temperature 55 DEG C insulation leave standstill 1 hour, mixed solution is layered as normal hexane layer and alcohol layer, is released by alcohol layer;
(4), normal hexane layer washes 3 times by step (2), (3);
(5), upper strata normal hexane layer clear water washs to pH=7;
(6), normal hexane layer is concentrated obtains xenthophylls 100kg, total lutein content 13476g, content yield 99.82%; Use high performance liquid phase to detect ethoxyquinoline, do not detect.
Embodiment 5
(1), 1000kg marigold flower particle through normal hexane extraction, filtration, concentrated after, obtain 180 liters of xenthophylls extracting solutions, detecting medicinal extract content through sampling is 58%, and total lutein content is 12600g, and in lutein extract, ethoxyquinoline content is 350ppb;
(2), in xenthophylls extracting solution, add the methanol solution (methanol solution citric acid adjust pH to 2.0) of 450 liters of volume fractions 30%, stir 40 minutes in 42 DEG C, obtain mixed solution;
(3), mixed solution in the separator temperature 42 DEG C insulation leave standstill 1 hour, mixed solution is layered as normal hexane layer and methanol layer, is released by methanol layer;
(4), normal hexane layer washes 4 times by step (2), (3);
(5), upper strata normal hexane layer clear water washs to pH=7;
(6), normal hexane layer is concentrated obtains xenthophylls 100kg, total lutein content 12540g, content yield 99.52%; Use high performance liquid phase to detect ethoxyquinoline, do not detect.
Above by embodiment to invention has been detailed description; but described content is only preferred embodiment of the present invention; utilize technical solutions according to the invention; or those skilled in the art is under the inspiration of technical solution of the present invention; design similar technical scheme; and reach above-mentioned technique effect, be all fall into protection scope of the present invention.

Claims (7)

1. the minimizing technology of ethoxyquinoline in lutein extract, is characterized in that, comprise the following steps:
(1) marigold flower particle is through normal hexane extraction, filtration, concentrating under reduced pressure, obtains xenthophylls extracting solution;
(2) in xenthophylls extracting solution, add the alcohol solution that pH value is 2-4, stir in 35-55 DEG C of water bath with thermostatic control and obtain mixed solution;
(3) layering: mixed solution, at temperature 35-55 DEG C, through centrifugal layering or stratification, is released lower floor's alcoholic solution layer, obtained upper strata normal hexane layer;
(4) wash: normal hexane layer clear water washing in upper strata is neutral to water layer pH;
(5) concentrated: normal hexane layer concentrates and namely obtains not containing the lutein extract of ethoxyquinoline.
2. the minimizing technology of ethoxyquinoline in a kind of lutein extract according to claim 1, it is characterized in that, the alcohol solution added in described step (2) is volume fraction is 30-60% methyl alcohol or aqueous ethanolic solution.
3. the minimizing technology of ethoxyquinoline in a kind of lutein extract according to claim 1, is characterized in that, be evaporated in described step (1) that lutein extract weight accounts for extracting liquid volume 30% ~ 70%.
4. in a kind of lutein extract according to claim 1-3 any one, the minimizing technology of ethoxyquinoline, is characterized in that, the alcohol solution phosphoric acid in described step (2), hydrochloric acid, citric acid adjust ph.
5. in a kind of lutein extract according to claim 1-3 any one, the minimizing technology of ethoxyquinoline, is characterized in that, in described step (2), the volume ratio of extracting solution and alcohol solution is 1:1-4.
6. in a kind of lutein extract according to claim 1-3 any one, the minimizing technology of ethoxyquinoline, is characterized in that, the water bath with thermostatic control in described step (2) is 35-55 DEG C, stirs 30-60min.
7. in a kind of lutein extract according to claim 1-3 any one, the minimizing technology of ethoxyquinoline, is characterized in that, the normal hexane layer obtained in described step (3) repeats 3-6 time according to step (2), (3) again.
CN201410656647.XA 2014-11-18 2014-11-18 The minimizing technology of ethoxyquinoline in a kind of lutein extract Active CN104387307B (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6191293B1 (en) * 1998-04-20 2001-02-20 Inexa, Industria Extractora C.A. Trans-xanthophyll ester concentrates of enhanced purity and methods of making same
WO2003037833A1 (en) * 2001-11-02 2003-05-08 Sobhanadri, Jonnalagadda Extraction of lutein from marigold meal
CN1436774A (en) * 2002-02-05 2003-08-20 海宁凤鸣叶绿素有限公司 Lutein crystal preparing process from marigold flower
EP1513804B1 (en) * 2002-06-05 2009-01-14 OmniActive Health Technologies Private Limited Novel trans-lutein enriched xanthophyll ester concentrate and a process for its preparation
CN101486671A (en) * 2009-02-27 2009-07-22 大连医诺生物有限公司 Preparation and stabilization of high-purity xanthophyll ester and method for removing pollutant thereof
CN102174005A (en) * 2011-01-25 2011-09-07 石河子大学医学院第一附属医院 Method for extracting lutein from marigold dried flowers
CN104059007A (en) * 2014-04-30 2014-09-24 西安岳达植物科技有限公司 Method for extracting lutein ester from marigold flowers

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6191293B1 (en) * 1998-04-20 2001-02-20 Inexa, Industria Extractora C.A. Trans-xanthophyll ester concentrates of enhanced purity and methods of making same
WO2003037833A1 (en) * 2001-11-02 2003-05-08 Sobhanadri, Jonnalagadda Extraction of lutein from marigold meal
CN1436774A (en) * 2002-02-05 2003-08-20 海宁凤鸣叶绿素有限公司 Lutein crystal preparing process from marigold flower
EP1513804B1 (en) * 2002-06-05 2009-01-14 OmniActive Health Technologies Private Limited Novel trans-lutein enriched xanthophyll ester concentrate and a process for its preparation
CN101486671A (en) * 2009-02-27 2009-07-22 大连医诺生物有限公司 Preparation and stabilization of high-purity xanthophyll ester and method for removing pollutant thereof
CN102174005A (en) * 2011-01-25 2011-09-07 石河子大学医学院第一附属医院 Method for extracting lutein from marigold dried flowers
CN104059007A (en) * 2014-04-30 2014-09-24 西安岳达植物科技有限公司 Method for extracting lutein ester from marigold flowers

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
刘洪海 等.万寿菊花钟叶黄素酯的提取及皂化工艺的研究.《农产品加工》.2009,(第3期),第71-74,77页. *
夏树林 等.从万寿菊中提取叶黄素的工艺研究.《安徽农业科学》.2006,第34卷(第19期),第5029-5030页. *

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Address after: 679100 shitoushan Industrial Park, Tengchong City, Baoshan City, Yunnan Province

Patentee after: Chenguang biotechnology group Tengchong Co., Ltd

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Patentee before: Chenguang Biotech Group Co.,Ltd.