CN106731006A - The method for separating and preparing of one Lepidopterous epoxy olefins isomer - Google Patents
The method for separating and preparing of one Lepidopterous epoxy olefins isomer Download PDFInfo
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- CN106731006A CN106731006A CN201611115286.3A CN201611115286A CN106731006A CN 106731006 A CN106731006 A CN 106731006A CN 201611115286 A CN201611115286 A CN 201611115286A CN 106731006 A CN106731006 A CN 106731006A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D301/00—Preparation of oxiranes
- C07D301/32—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
- C07D303/02—Compounds containing oxirane rings
- C07D303/04—Compounds containing oxirane rings containing only hydrogen and carbon atoms in addition to the ring oxygen atoms
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Abstract
HPLC separating and purifying technologies field is prepared the invention belongs to half, and in particular to the method for separating and preparing of a Lepidopterous epoxy olefins isomer, comprise the following steps：1）The preparation of semi-preparative liquid chromatography；2）The preparation of mobile phase；3）Mobile phase parameter setting；4）Sample is separated and prepared.The present invention can efficiently separate artificial synthesized C17‑C23Epoxy olefins isomeric mixtures, with preparation amount it is big, purity is high the characteristics of.
Description
Technical field
HPLC separating and purifying technologies field is prepared the invention belongs to half, and in particular to a Lepidopterous epoxy olefins are different with dividing
The method for separating and preparing of structure body.
Background technology
Insect sex pheromone, is by a certain sex of insect of the same race individual special secretory point also known as extra-sexual hormone
Secrete in external, can be received by the individual receptor of the opposite sex of the same race, and cause the certain behavior reaction of different in nature individual generation or life
Reason effect（Even, orientation is such as looked for seek a spouse, mate）Trace level chemical substance.Insect sex pheromone is used as the chemistry sixties in last century
Ecological important discovery, because it has the advantages that efficient, environmentally friendly, selectivity is strong, by the affirmative of scientists from all over the world, is considered as
It is " biorational pesticides ".Report more than the 600 kinds of lepidopterous insects sex pheromone identified according to chemical constitution feature base at present
Originally 3 big types can be summarized as.The sex pheromone of Class1 is C10-C18Unsaturated Long carbon chain structure, carbochain end have hydroxyl,
The functional groups such as formoxyl, acetyl group, are common in the sex pheromone composition of the moth class such as Crambidae, Tortricidae and Noctuidae.Type 2
Sex pheromone is C17-C23Alkene and its epoxides, such sex pheromone chemical constitution is relative complex, is more common in looper
Section, Lymantriidae and Arctiidae.The middle carbon potential that the sex pheromone of type 3 is mainly characterized by Long carbon chain has the chemistry knot such as methyl
Structure, such chemical structure information element is comparatively rare.
The current sex pheromone artificial synthesis of Lepidoptera type 2 are main corresponding as substrate synthesis with leukotrienes or linoleic acid
Triolefin or diene, then with gained olefin oxidation.Due to being random oxidation, therefore ring in the double bond of triolefin or diene
Oxygen olefin product is equivalent isomeric mixtures, and the product after such as cis- 3,6,9- ten eight carbon triolefin oxidations is cis- the 6 of equivalent,
The carbon diene of 9- epoxies -3,4- 18, the cis- carbon diene of 3,9- epoxies -6,7- 18 and the cis- carbon two of 3,6- epoxies -9,10- 18
Alkene.Found in the application study of sex pheromone, the epoxy olefins isomer of part lepidopterous insects has inhibition letter
The phenomenon of breath element activity, therefore can efficiently separate the method for preparing epoxy olefins isomer in the urgent need to exploitation is a kind of.
The content of the invention
In order to make up the deficiencies in the prior art, the technical problems to be solved by the invention are to provide a Lepidopterous epoxy alkene
The method for separating and preparing of hydrocarbon isomer, the present invention can efficiently separate artificial synthesized C17-C23Epoxy olefins isomerism
Mixture, with preparation amount it is big, purity is high the characteristics of.
In order to solve the above technical problems, the present invention provides the separation preparation side of a Lepidopterous epoxy olefins isomer
Method, comprises the following steps：
1）The preparation of semi-preparative liquid chromatography：It is sequentially connected four source gradient modules, automatic sampler, detector and fraction collection
Device, installs ultrapure silica gel positive preparative chromatography post, and the ultrapure silica gel positive preparative chromatography column parameter is：Granularity particle diameter 5-10
Micron, column diameter 10-50 millimeters, column's length 50-250 millimeters；
2）The preparation of mobile phase：N-hexane 50-99 parts by volume and tetrahydrofuran 0.25-20 parts by volume are measured respectively, by tetrahydrochysene furan
Mutter in addition n-hexane, mixing is placed in ultrasound 5 minutes in ultrasonic sound appratus；
3）By step 2）The flowing of middle preparation is connected into semi-preparative liquid chromatography, sets the inspection of semi-preparative liquid chromatography detector
It is 190-280 nanometers to survey wavelength, and flow rate of mobile phase is 0.5-10 liters/min；
4）Lepidoptera epoxy olefins admixture of isomeric compound sample to be separated is placed in automatic sampler, sample size is set
And run time, you can isomer cut is collected in fraction collector.
Further, the ultrapure silica gel positive preparative chromatography column parameter is：10 microns of granularity particle diameter, column diameter
30-50 millimeters and column's length 100-250 millimeters；N-hexane is that 75-99 parts by volume, tetrahydrofuran are in the mobile phase
10-20 parts by volume；The Detection wavelength of the semi-preparative liquid chromatography detector is 235-280 nanometers, and flow rate of mobile phase is 5-10
Liter/min.
Further, the ultrapure silica gel positive preparative chromatography column parameter is：5 microns of granularity particle diameter, column diameter
10-30 millimeters and column's length 50-100 millimeters；N-hexane is that 50-75 parts by volume, tetrahydrofuran are in the mobile phase
0.25-10 parts by volume；The Detection wavelength of the semi-preparative liquid chromatography detector is 190-235 nanometers, and flow rate of mobile phase is
0.5-5 liters/min.
Further, the ultrapure silica gel positive preparative chromatography column parameter is：5 microns of granularity particle diameter, column diameter
20-40 millimeters and column's length 70-150 millimeters；In the mobile phase n-hexane be 60-80 parts by volume, tetrahydrofuran be 5-
15 parts by volume；The Detection wavelength of the semi-preparative liquid chromatography detector is 220-250 nanometers, and flow rate of mobile phase is 2-8 liters/min
Clock.
Beneficial effect of the present invention：The present invention can provide one kind and can efficiently separate, and possess the Lepidoptera of doses scale
Epoxy olefins isomer.The present invention suitably prepares post and stream with semi-preparative liquid chromatography as separate apparatus by selection
Dynamic phase, to artificial synthesized C under specific flow rate of mobile phase and wavelength detecting17-C23Epoxy olefins isomerism mixing
Thing reaches and efficiently separates, and relative to other conventional separation methods, the present invention has the characteristics of preparation amount is big, purity is high.Purifying
Lepidoptera epoxy olefins afterwards can be used to make sex pheromone lure core, be applied to population monitoring and the preventing and treating of lepidopterous insects,
And it is pollution-free, environment-friendly.Additionally, the present invention can also provide technology branch for the commercial application of lepidopterous insects sex pheromone
Hold, have broad application prospects.
Brief description of the drawings
Fig. 1 separates figure for artificial synthesized grey tea geometrid sex pheromone epoxy olefins admixture of isomeric compound；
Fig. 2 is the mass spectrogram of the cis- carbon diene of 6,9- epoxies -3,4- 18；
Fig. 3 is the mass spectrogram of the cis- carbon diene of 3,9- epoxies -6,7- 18；
Fig. 4 is the mass spectrogram of the cis- carbon diene of 3,6- epoxies -9,10- 18.
Specific embodiment
The present invention is further described in detail with reference to specific embodiment.Heretofore described embodiment is only used for
It is bright to explain the present invention without being construed as limiting to the scope of the present invention.
Embodiment 1:
The method for separating and preparing of one Lepidopterous epoxy olefins isomer, it is characterised in that comprise the following steps：
1）The preparation of semi-preparative liquid chromatography：It is sequentially connected four source gradient modules, automatic sampler, detector and fraction collection
Device, installs ultrapure silica gel positive preparative chromatography post, and the ultrapure silica gel positive preparative chromatography column parameter is：Granularity particle diameter 5 is micro-
Rice, 10 millimeters of column diameter, 50 millimeters of column's length；
2）The preparation of mobile phase：The parts by volume of n-hexane 50 and the parts by volume of tetrahydrofuran 0.25 are measured respectively, and tetrahydrofuran is added
In n-hexane, mixing is placed in ultrasound 5 minutes in ultrasonic sound appratus；
3）By step 2）The flowing of middle preparation is connected into semi-preparative liquid chromatography, sets the inspection of semi-preparative liquid chromatography detector
It is 190 nanometers to survey wavelength, and flow rate of mobile phase is 0.5 liter/min；
4）Lepidoptera epoxy olefins admixture of isomeric compound sample to be separated is placed in automatic sampler, sample size is set
And run time, you can isomer cut is collected in fraction collector.
Embodiment 2：
The method for separating and preparing of one Lepidopterous epoxy olefins isomer, it is characterised in that comprise the following steps：
1）The preparation of semi-preparative liquid chromatography：It is sequentially connected four source gradient modules, automatic sampler, detector and fraction collection
Device, installs ultrapure silica gel positive preparative chromatography post, and the ultrapure silica gel positive preparative chromatography column parameter is：Granularity particle diameter 5 is micro-
Rice, 19 millimeters of column diameter, 75 millimeters of column's length；
2）The preparation of mobile phase：Measure the parts by volume of n-hexane 60 and the parts by volume of tetrahydrofuran 5 respectively, by tetrahydrofuran add just oneself
In alkane, mixing is placed in ultrasound 5 minutes in ultrasonic sound appratus；
3）By step 2）The flowing of middle preparation is connected into semi-preparative liquid chromatography, sets the inspection of semi-preparative liquid chromatography detector
It is 200 nanometers to survey wavelength, and flow rate of mobile phase is 1 liter/min；
4）Lepidoptera epoxy olefins admixture of isomeric compound sample to be separated is placed in automatic sampler, sample size is set
And run time, you can isomer cut is collected in fraction collector.
Embodiment 3：
The method for separating and preparing of one Lepidopterous epoxy olefins isomer, it is characterised in that comprise the following steps：
1）The preparation of semi-preparative liquid chromatography：It is sequentially connected four source gradient modules, automatic sampler, detector and fraction collection
Device, installs ultrapure silica gel positive preparative chromatography post, and the ultrapure silica gel positive preparative chromatography column parameter is：Granularity particle diameter 5 is micro-
Rice, 30 millimeters of column diameter, 100 millimeters of column's length；
2）The preparation of mobile phase：The parts by volume of n-hexane 75 and the parts by volume of tetrahydrofuran 10 are measured respectively, and tetrahydrofuran is added just
In hexane, mixing is placed in ultrasound 5 minutes in ultrasonic sound appratus；
3）By step 2）The flowing of middle preparation is connected into semi-preparative liquid chromatography, sets the inspection of semi-preparative liquid chromatography detector
It is 215 nanometers to survey wavelength, and flow rate of mobile phase is 3 liters/min；
4）Lepidoptera epoxy olefins admixture of isomeric compound sample to be separated is placed in automatic sampler, sample size is set
And run time, you can isomer cut is collected in fraction collector.
Embodiment 4
The method for separating and preparing of one Lepidopterous epoxy olefins isomer, it is characterised in that comprise the following steps：
1）The preparation of semi-preparative liquid chromatography：It is sequentially connected four source gradient modules, automatic sampler, detector and fraction collection
Device, installs ultrapure silica gel positive preparative chromatography post, and the ultrapure silica gel positive preparative chromatography column parameter is：Granularity particle diameter 10 is micro-
Rice, 50 millimeters of column diameter, 150 millimeters of column's length；
2）The preparation of mobile phase：The parts by volume of n-hexane 75 and the parts by volume of tetrahydrofuran 10 are measured respectively, and tetrahydrofuran is added just
In hexane, mixing is placed in ultrasound 5 minutes in ultrasonic sound appratus；
3）By step 2）The flowing of middle preparation is connected into semi-preparative liquid chromatography, sets the inspection of semi-preparative liquid chromatography detector
It is 215 nanometers to survey wavelength, and flow rate of mobile phase is 3 liters/min；
4）Lepidoptera epoxy olefins admixture of isomeric compound sample to be separated is placed in automatic sampler, sample size is set
And run time, you can isomer cut is collected in fraction collector.
Embodiment 5
The method for separating and preparing of one Lepidopterous epoxy olefins isomer, it is characterised in that comprise the following steps：
1）The preparation of semi-preparative liquid chromatography：It is sequentially connected four source gradient modules, automatic sampler, detector and fraction collection
Device, installs ultrapure silica gel positive preparative chromatography post, and the ultrapure silica gel positive preparative chromatography column parameter is：Granularity particle diameter 10 is micro-
Rice, 50 millimeters of column diameter, 150 millimeters of column's length；
2）The preparation of mobile phase：The parts by volume of n-hexane 85 and the parts by volume of tetrahydrofuran 15 are measured respectively, and tetrahydrofuran is added just
In hexane, mixing is placed in ultrasound 5 minutes in ultrasonic sound appratus；
3）By step 2）The flowing of middle preparation is connected into semi-preparative liquid chromatography, sets the inspection of semi-preparative liquid chromatography detector
It is 250 nanometers to survey wavelength, and flow rate of mobile phase is 5 liters/min；
4）Lepidoptera epoxy olefins admixture of isomeric compound sample to be separated is placed in automatic sampler, sample size is set
And run time, you can isomer cut is collected in fraction collector.
Embodiment 6
The method for separating and preparing of one Lepidopterous epoxy olefins isomer, it is characterised in that comprise the following steps：
1）The preparation of semi-preparative liquid chromatography：It is sequentially connected four source gradient modules, automatic sampler, detector and fraction collection
Device, installs ultrapure silica gel positive preparative chromatography post, and the ultrapure silica gel positive preparative chromatography column parameter is：Granularity particle diameter 10 is micro-
Rice, 50 millimeters of column diameter, 250 millimeters of column's length；
2）The preparation of mobile phase：The parts by volume of n-hexane 75 and the parts by volume of tetrahydrofuran 10 are measured respectively, and tetrahydrofuran is added just
In hexane, mixing is placed in ultrasound 5 minutes in ultrasonic sound appratus；
3）By step 2）The flowing of middle preparation is connected into semi-preparative liquid chromatography, sets the inspection of semi-preparative liquid chromatography detector
It is 215 nanometers to survey wavelength, and flow rate of mobile phase is 3 liters/min；
4）Lepidoptera epoxy olefins admixture of isomeric compound sample to be separated is placed in automatic sampler, sample size is set
And run time, you can isomer cut is collected in fraction collector.
Embodiment 7
The method for separating and preparing of one Lepidopterous epoxy olefins isomer, it is characterised in that comprise the following steps：
1）The preparation of semi-preparative liquid chromatography：It is sequentially connected four source gradient modules, automatic sampler, detector and fraction collection
Device, installs ultrapure silica gel positive preparative chromatography post, and the ultrapure silica gel positive preparative chromatography column parameter is：Granularity particle diameter 10 is micro-
Rice, 50 millimeters of column diameter, 250 millimeters of column's length；
2）The preparation of mobile phase：The parts by volume of n-hexane 99 and the parts by volume of tetrahydrofuran 20 are measured respectively, and tetrahydrofuran is added just
In hexane, mixing is placed in ultrasound 5 minutes in ultrasonic sound appratus；
3）By step 2）The flowing of middle preparation is connected into semi-preparative liquid chromatography, sets the inspection of semi-preparative liquid chromatography detector
It is 280 nanometers to survey wavelength, and flow rate of mobile phase is 10 liters/min；
4）Lepidoptera epoxy olefins admixture of isomeric compound sample to be separated is placed in automatic sampler, sample size is set
And run time, you can isomer cut is collected in fraction collector.
It should be noted that, sample size and run time are set according to the property of target compound in the present invention, this hair
The concrete operations and step being not written out in bright belong to this area conventional technical means.
Test example：
Cis- 3,9- epoxy -6, the carbon diene of 7- 18 is one of grey tea geometrid sex pheromone composition, in the mistake of its artificial chemistry synthesis
Cheng Zhong, with cis- 3,6,9- ten eight carbon triolefins for the epoxidation step of substrate in, generate cis- 6,9- epoxy -3 of equivalent, 4- ten
Eight carbon diene, the cis- carbon diene of 3,9- epoxies -6,7- 18 and the cis- carbon diene of 3,6- epoxies -9,10- 18.This test example is used
The method of the invention carries out separation preparation to above-mentioned epoxy olefins admixture of isomeric compound.Gained mixture is dissolved in first
N-hexane, be configured to 10 micrograms/microlitre sample, be placed in half preparation HPLC automatic samplers.Then reality of the present invention is pressed
Apply the step of example 3 and separate preparation.
From figure 1 it appears that can completely by artificial synthesized grey tea geometrid sex pheromone using the method for the invention
Three kinds of epoxy olefins isomers be kept completely separate, wherein cis- 6,9- epoxy -3, the appearance time of the carbon diene of 4- 18 is
34.0-36.0 minutes, cis- 3,9- epoxy -6, the appearance time of the carbon diene of 7- 18 is 28.5-33.5 minutes, cis- 3,6- rings
Oxygen -9, the appearance time of the carbon diene of 10- 18 is 36.5-40.5 minutes, wherein cis- 3,9- epoxy -6, the carbon diene of 7- 18 without
UV absorption, therefore cut is further verified by GC-MS.Fig. 2, Fig. 3 and Fig. 4 are respectively cis- 6,9- epoxies -3,4- 18
The mass spectrogram of carbon diene, the cis- carbon diene of 3,9- epoxies -6,7- 18 and the cis- carbon diene of 3,6- epoxies -9,10- 18.Thus may be used
See, preparation method of the present invention has good separating effect, and the purity of prepared sample is also higher.
Claims (4)
1. the method for separating and preparing of a Lepidopterous epoxy olefins isomer, it is characterised in that comprise the following steps：
1）The preparation of semi-preparative liquid chromatography：It is sequentially connected four source gradient modules, automatic sampler, detector and fraction collection
Device, installs ultrapure silica gel positive preparative chromatography post, and the ultrapure silica gel positive preparative chromatography column parameter is：Granularity particle diameter 5-10
Micron, column diameter 10-50 millimeters and column's length 50-250 millimeters；
2）The preparation of mobile phase：N-hexane 50-99 parts by volume and tetrahydrofuran 0.25-20 parts by volume are measured respectively, by tetrahydrochysene furan
Mutter in addition n-hexane, mixing is placed in ultrasound 5 minutes in ultrasonic sound appratus；
3）By step 2）The flowing of middle preparation is connected into semi-preparative liquid chromatography, sets the inspection of semi-preparative liquid chromatography detector
It is 190-280 nanometers to survey wavelength, and flow rate of mobile phase is 0.5-10 liters/min；
4）Lepidoptera epoxy olefins admixture of isomeric compound sample to be separated is placed in automatic sampler, sample size is set
And run time, you can isomer cut is collected in fraction collector.
2. the method for separating and preparing of Lepidopterous epoxy olefins isomer according to claim 1, its feature exists
It is in the ultrapure silica gel positive preparative chromatography column parameter：10 microns, column diameter 30-50 millimeters of granularity particle diameter and chromatogram
100-250 millimeters of post column length；In the mobile phase n-hexane be 75-99 parts by volume, tetrahydrofuran be 10-20 parts by volume；It is described
The Detection wavelength of semi-preparative liquid chromatography detector is 235-280 nanometers, and flow rate of mobile phase is 5-10 liters/min.
3. the method for separating and preparing of Lepidopterous epoxy olefins isomer according to claim 1, its feature exists
It is in the ultrapure silica gel positive preparative chromatography column parameter：5 microns, column diameter 10-30 millimeters of granularity particle diameter and chromatogram
50-100 millimeters of post column length；In the mobile phase n-hexane be 50-75 parts by volume, tetrahydrofuran be 0.25-10 parts by volume；It is described
The Detection wavelength of semi-preparative liquid chromatography detector is 190-235 nanometers, and flow rate of mobile phase is 0.5-5 liters/min.
4. the method for separating and preparing of Lepidopterous epoxy olefins isomer according to claim 1, its feature exists
It is in the ultrapure silica gel positive preparative chromatography column parameter：5 microns, column diameter 20-40 millimeters of granularity particle diameter and chromatogram
70-150 millimeters of post column length；In the mobile phase n-hexane be 60-80 parts by volume, tetrahydrofuran be 5-15 parts by volume；Described half
The Detection wavelength of preparative liquid chromatography detector is 220-250 nanometers, and flow rate of mobile phase is 2-8 liters/min.
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| CN201611115286.3A CN106731006A (en) | 2016-12-07 | 2016-12-07 | The method for separating and preparing of one Lepidopterous epoxy olefins isomer |
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| CN201611115286.3A CN106731006A (en) | 2016-12-07 | 2016-12-07 | The method for separating and preparing of one Lepidopterous epoxy olefins isomer |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1289922A (en) * | 2000-11-21 | 2001-04-04 | 中国人民解放军军事医学科学院放射医学研究所 | Biochemical Process for preparing liquid-phase chromatograph |
| US20110184658A1 (en) * | 2008-08-19 | 2011-07-28 | Shimadzu Corporation | Preparative Liquid Chromatograph System |
| CN203224485U (en) * | 2013-05-24 | 2013-10-02 | 江苏迪沃特仪器设备科技有限公司 | Liquid phase semipreparative all-in-one machine |
| CN106053692A (en) * | 2016-07-29 | 2016-10-26 | 颜海 | Method for splitting amlodipine antimer by high-performance liquid chromatography |
-
2016
- 2016-12-07 CN CN201611115286.3A patent/CN106731006A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1289922A (en) * | 2000-11-21 | 2001-04-04 | 中国人民解放军军事医学科学院放射医学研究所 | Biochemical Process for preparing liquid-phase chromatograph |
| US20110184658A1 (en) * | 2008-08-19 | 2011-07-28 | Shimadzu Corporation | Preparative Liquid Chromatograph System |
| CN203224485U (en) * | 2013-05-24 | 2013-10-02 | 江苏迪沃特仪器设备科技有限公司 | Liquid phase semipreparative all-in-one machine |
| CN106053692A (en) * | 2016-07-29 | 2016-10-26 | 颜海 | Method for splitting amlodipine antimer by high-performance liquid chromatography |
Non-Patent Citations (2)
| Title |
|---|
| TETSU ANDO等: "sex attractants of geometrid and noctuid moths：chemical characterization and field test of nomoepoxides of 6,9-dienes and related compounds", 《JOURNAL OF CHEMICAL ECOLOGY》 * |
| 冯年平等主编: "《中药提取分离技术原理与应用》", 28 February 2005, 中国医药科技出版社 * |
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Application publication date: 20170531 |