CN107843659A - A kind of solution positive liquid chromatographic detection pyrethrin pesticide aqueous emulsion and aqueous suspension agent and the immiscible method of solvent - Google Patents
A kind of solution positive liquid chromatographic detection pyrethrin pesticide aqueous emulsion and aqueous suspension agent and the immiscible method of solvent Download PDFInfo
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- CN107843659A CN107843659A CN201710919119.2A CN201710919119A CN107843659A CN 107843659 A CN107843659 A CN 107843659A CN 201710919119 A CN201710919119 A CN 201710919119A CN 107843659 A CN107843659 A CN 107843659A
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- G01N30/02—Column chromatography
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a kind of solution positive liquid chromatographic detection pyrethrin pesticide aqueous emulsion and aqueous suspension agent and the immiscible method of solvent, it is related to Pesticides Testing technical field, a kind of cosolvent is added in detection method, co-solvent components are：Ethylenediamine, salicylic acid, glycine, 70% methanol aqueous solution；Wherein cosolvent has security, feasibility, validity, and preparation method is simple to operation, when detecting pyrethrin pesticide aqueous emulsion and aqueous suspension agent, it is easy to use, on stability of drug products without influence, pyrethrin pesticide aqueous emulsion and aqueous suspension agent is set to be mixed with solvent, rate of recovery when can effectively improve the degree of accuracy in detection, testing result is met Theoretical Prediction numerical value, reach the needs of detection.
Description
Technical field：
The present invention relates to Pesticides Testing technical field, and in particular to normal phase liquid chromatography detects pyrethrin pesticide aqueous emulsion
With the detection method of aqueous suspension agent.
Background technology：
Chemical pesticide has made outstanding contributions for agricultural volume increase and increasing peasant income for a long time, but because the mankind are to chemistry
The unreasonable use of agricultural chemicals, increases pesticide residue in agricultural products, and environmental pollution is serious, while jeopardizes human health and life
Life.Into 21 century, with the continuous enhancing of people's environmental consciousness and security knowledge, research and development " water-based, granular, sustained release,
It is multi-functional, Labor-saving and become more meticulous " the formulations of pesticide turn into focus both domestic and external.The good water-based pesticides system of Environmental compatibility
Agent has been to be concerned by more and more people, and this kind of preparation mainly includes aqueous suspension agent (Suspension concentrate, SC), micro-
Capsule aqueous suspension agent (Capsule suspension, CS), aqueous emulsion (Emulsion, EW), microemulsion (Micro emulsion,
ME) and aqua (Aqueous solution, AS) etc. [4], have and save organic solvent, reduce environmental pollution, to people and animals' phase
To safety, the advantages that cost is relatively low.Pesticide suspension concentrate is due to its good Environmental compatibility, drug effect is high, cost is low and processing
It is safe to use, show one's talent in water-based aerosol, there is very big development potentiality.
But chemical pesticide is in process of production, it is necessary to various quality testings, to ensure chemical pesticide safety and effectiveness；And
In the detection of liquid chromatogram positive, solvent for use and mobile phase are all oil-based solvents, when running into aqueous emulsion and aqueous suspension agent, though through
Sonic oscillation and shake, sample can not lump together with solvent all the time.So when producing chrysanthemum esters aqueous emulsion and aqueous suspension agent,
Testing result is always relatively low in Theoretical Prediction numerical value, and when doing the degree of accuracy, the rate of recovery can only not reach preferably 95% or so
It is required that.
The content of the invention：
The technical problems to be solved by the invention are to provide a kind of solution positive liquid chromatographic detection pyrethrin pesticide water
Emulsion and aqueous suspension agent and the immiscible method of solvent, pyrethrin pesticide aqueous emulsion and aqueous suspension agent can mix with solvent, examine
Survey result and meet Theoretical Prediction numerical value, the rate of recovery can reach more than 96% when doing the degree of accuracy, reach preferable requirement.
By largely testing, find to add a certain amount of cosolvent to improve the intermiscibility of sample system, make effectively into
Divide and be uniformly dissolved, reach the needs of detection.Tested by accuracy, its rate of recovery reaches promising result.Reaffirm it is sample
It is not high with the intermiscibility of solvent, and cause accuracy to reduce.
The technical problems to be solved by the invention are realized using following technical scheme：
A kind of cosolvent, its composition include：Ethylenediamine, salicylic acid, glycine, 70% methanol aqueous solution.
Wherein described ethylenediamine, salicylic acid, glycine, ethylenediamine：Salicylic acid：Glycine is according to 0.1:1:0.5~0.5:
1.0:0.8 carries out being configured to cosolvent basal liquid；
70% methanol aqueous solution is added in backward basal liquid, wherein 70% methanol aqueous solution：Basal liquid=7:3；
Cosolvent preparation method is：
(1) by ethylenediamine：Salicylic acid：Glycine is according to 0.1:1.0:0.2~0.5:1.0:0.6 ratio precision weighing, will
Ethylenediamine, salicylic acid are placed in precision weighing in glass beaker, three after exact value decimal point；Glycine is placed on pan paper again
Precision weighing, after the glycine of weighing is placed in ethylenediamine, salicylic acid is placed in glass beaker；
(2) first step 1 beaker being placed on heating magnetic stirring apparatus in ventilating kitchen, slow heating is warming up to 40 DEG C, and
200-600rpm/min is stirred, and is well mixed；
(3) by 70% methanol aqueous solution with no more than 70% methanol aqueous solution after：Basal liquid (V7:3) ratio, step is added
In rapid 2 mixed liquor, continue to heat 200-600rpm/min stirrings, until mixture is completely dissolved；
(4) step 3 mixed liquor is added in volumetric flask, 70% methanol aqueous solution is added in backward volumetric flask, until 70%
Methanol aqueous solution：Basal liquid (V7:3)；
(5) solution bottle,suction after step 4 constant volume and 0.45 μm of organic filter membrane are filtered 2 times, pressure 0.1Mpa, removed
Impurity in mixed liquor；
(6) solution after suction filtration is fitted into after totally sterilizing in blue mouth bottle, bottle cap is not easy to tighten, and bottle cap easily covers；
(7) blue lid bottle of the step 6 equipped with mixed liquor is placed in ultrasonic 5-15min in ultrafilter after, ultrasound terminate after by indigo plant
Lid bottle is tightened and is positioned over 0-4 DEG C of reagent storage refrigerator.
Positive liquid chromatographic detection pyrethrin pesticide aqueous emulsion and aqueous suspension agent process：
In normal phase high performance liquid chromatography detection process, using 2.5% efficient chlorine fluorine cyanogen aqueous emulsion as detection sample, specific inspection
Survey method is as follows：
(1) instrument and reagent
The type high performance liquid chromatograph of Agilent 1260, Variable wavelength UV detector, N2000 work stations, filter, ultrasound
Ripple washer；
Methanol (chromatographic grade), acetonitrile (chromatographic grade), deionized water, efficient chlorine fluorine cyanogen aqueous emulsion.
(2) preparation of standard specimen solution
Gamma cyhalothrin standard sample 0.03g (being accurate to 0.0002g) is weighed in 50mL volumetric flasks, with 70% first
Alcohol solution dissolves and is diluted to scale, sonic oscillation 5min, removes recovery to room temperature, standby.
(3) preparation of sample solution
2.5% efficient chlorine fluorine cyanogen aqueous emulsion 0.03g sample (being accurate to 0.0002g) is weighed in 50mL volumetric flasks, is added
Enter 1-3g anhydrous sodium sulfates, then accurate addition cosolvent, wherein rear accurate addition 70% methanol aqueous solution dissolving, cosolvent：
70% methanol aqueous solution is 1:5-10, sonic oscillation 5-10min, recovery is removed to room temperature, has millipore filter mistake through 0.45 μm
Filter, filtrate are to be measured.
(4) chromatographiccondition
Chromatographic column：250mm × 6.5mm, 5 μm, WandaSilC18 posts；25 ± 1 DEG C of column temperature；Mobile phase：Methanol：Acetonitrile：Water
(V 30:40:30), flow velocity 0.5-1.0ml/min；Detection wavelength 235nm；Sampling volume： 10μl.
The beneficial effects of the invention are as follows：A kind of solution positive liquid chromatographic detection pyrethrin pesticide aqueous emulsion of the present invention
With aqueous suspension agent and the immiscible method of solvent, wherein cosolvent has security, feasibility, validity, and preparation method letter
It is single easy to operate, it is easy to use when detecting pyrethrin pesticide aqueous emulsion and aqueous suspension agent, on stability of drug products without influence, make chrysanthemum
Ester pesticides aqueous emulsion and aqueous suspension agent can mix with solvent, rate of recovery when can effectively improve the degree of accuracy in detection, make
Testing result meets Theoretical Prediction numerical value, reaches the needs of detection.
Embodiment：
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment 1：
The technical problems to be solved by the invention are realized using following technical scheme：
A kind of cosolvent, its composition include：Ethylenediamine, salicylic acid, glycine, 70% methanol aqueous solution.
Wherein described ethylenediamine, salicylic acid, glycine, ethylenediamine：Salicylic acid：Glycine is according to 0.1:1:0.5 is matched somebody with somebody
Cosolvent basal liquid is made；
70% methanol aqueous solution is added in backward basal liquid, wherein 70% methanol aqueous solution：Basal liquid=7:3；
Cosolvent preparation method is：
(1) by ethylenediamine：Salicylic acid：Glycine is according to 0.1:1.0:0.2 ratio precision weighing, by ethylenediamine, salicylic acid
Precision weighing in glass beaker is placed in, three after exact value decimal point；Glycine is placed in precision weighing on pan paper again, after will
The glycine of weighing is placed in ethylenediamine, and salicylic acid is placed in glass beaker；
(2) first step 1 beaker being placed on heating magnetic stirring apparatus in ventilating kitchen, slow heating is warming up to 40 DEG C, and
500rpm/min is stirred, and is well mixed；
(3) by 70% methanol aqueous solution with no more than 70% methanol aqueous solution after：Basal liquid (V7:3) ratio, step is added
In rapid 2 mixed liquor, continue to heat 500rpm/min stirrings, until mixture is completely dissolved；
(4) step 3 mixed liquor is added in volumetric flask, 70% methanol aqueous solution is added in backward volumetric flask, until 70%
Methanol aqueous solution：Basal liquid (V7:3)；
(5) solution bottle,suction after step 4 constant volume and 0.45 μm of organic filter membrane are filtered 2 times, pressure 0.1Mpa, removed
Impurity in mixed liquor；
(6) solution after suction filtration is fitted into after totally sterilizing in blue mouth bottle, bottle cap is not easy to tighten, and bottle cap easily covers；
(7) blue lid bottle of the step 6 equipped with mixed liquor is placed in ultrasonic 10min in ultrafilter after, ultrasound covers indigo plant after terminating
Bottle is tightened and is positioned over 4 DEG C of reagent storage refrigerators.
Positive liquid chromatographic detection pyrethrin pesticide aqueous emulsion process：
In normal phase high performance liquid chromatography detection process, using 2.5% efficient chlorine fluorine cyanogen aqueous emulsion as detection sample, specific inspection
Survey method is as follows：
(2) instrument and reagent
The type high performance liquid chromatograph of Agilent 1260, Variable wavelength UV detector, N2000 work stations, filter, ultrasound
Ripple washer；
Methanol (chromatographic grade), acetonitrile (chromatographic grade), deionized water, efficient chlorine fluorine cyanogen aqueous emulsion.
(2) preparation of standard specimen solution
Gamma cyhalothrin standard sample 0.03g (being accurate to 0.0002g) is weighed in 50mL volumetric flasks, with 70% first
Alcohol solution dissolves and is diluted to scale, sonic oscillation 5min, removes recovery to room temperature, standby.
(3) preparation of sample solution
2.5% efficient chlorine fluorine cyanogen aqueous emulsion 0.03g sample (being accurate to 0.0002g) is weighed in 50mL volumetric flasks, is added
Enter 3g anhydrous sodium sulfates, then accurate addition cosolvent, wherein rear accurate addition 70% methanol aqueous solution dissolving, cosolvent：70%
Methanol aqueous solution is 1:5, sonic oscillation 5min, recovery is removed to room temperature, has millipore filter filtering through 0.45 μm, filtrate is treated
Survey.
(4) chromatographiccondition
Chromatographic column：250mm × 6.5mm, 5 μm, WandaSilC18 posts；25 ± 1 DEG C of column temperature；Mobile phase：Methanol：Acetonitrile：Water
(V 30:40:30), flow velocity 1.0ml/min；Detection wavelength 235nm；Sampling volume： 10μl.
Wherein contrast experiment is tested with being not added with cosolvent, and testing result is as follows：Table 2 (does not add cosolvent)；Table 3
(addition cosolvent)；
The gamma cyhalothrin aqueous emulsion assay method accuracy test of table 2
The gamma cyhalothrin aqueous emulsion assay method accuracy test of table 3
Embodiment 2：
The technical problems to be solved by the invention are realized using following technical scheme：
A kind of cosolvent, its composition include：Ethylenediamine, salicylic acid, glycine, 70% methanol aqueous solution.
Wherein described ethylenediamine, salicylic acid, glycine, ethylenediamine：Salicylic acid：Glycine is according to 0.1:1:0.5 is matched somebody with somebody
Cosolvent basal liquid is made；
70% methanol aqueous solution is added in backward basal liquid, wherein 70% methanol aqueous solution：Basal liquid=7:3；
Cosolvent preparation method is：
(1) by ethylenediamine：Salicylic acid：Glycine is according to 0.1:1.0:0.2 ratio precision weighing, by ethylenediamine, salicylic acid
Precision weighing in glass beaker is placed in, three after exact value decimal point；Glycine is placed in precision weighing on pan paper again, after will
The glycine of weighing is placed in ethylenediamine, and salicylic acid is placed in glass beaker；
(2) first step 1 beaker being placed on heating magnetic stirring apparatus in ventilating kitchen, slow heating is warming up to 40 DEG C, and
450rpm/min is stirred, and is well mixed；
(3) by 70% methanol aqueous solution with no more than 70% methanol aqueous solution after：Basal liquid (V7:3) ratio, step is added
In rapid 2 mixed liquor, continue to heat 400rpm/min stirrings, until mixture is completely dissolved；
(4) step 3 mixed liquor is added in volumetric flask, 70% methanol aqueous solution is added in backward volumetric flask, until 70%
Methanol aqueous solution：Basal liquid (V7:3)；
(5) solution bottle,suction after step 4 constant volume and 0.45 μm of organic filter membrane are filtered 2 times, pressure 0.1Mpa, removed
Impurity in mixed liquor；
(6) solution after suction filtration is fitted into after totally sterilizing in blue mouth bottle, bottle cap is not easy to tighten, and bottle cap easily covers；
(7) blue lid bottle of the step 6 equipped with mixed liquor is placed in ultrasonic 15min in ultrafilter after, ultrasound covers indigo plant after terminating
Bottle is tightened and is positioned over 4 DEG C of reagent storage refrigerators.
Positive liquid chromatographic detection pyrethrin pesticide aqueous suspension agent process：
In normal phase high performance liquid chromatography detection process, using 2.5% efficient chlorine fluorine cyanogen aqueous suspension agent as detection sample, specifically
Detection method is as follows：
(3) instrument and reagent
The type high performance liquid chromatograph of Agilent 1260, Variable wavelength UV detector, N2000 work stations, filter, ultrasound
Ripple washer；
Methanol (chromatographic grade), acetonitrile (chromatographic grade), deionized water, efficient chlorine fluorine cyanogen aqueous emulsion.
(2) preparation of standard specimen solution
Gamma cyhalothrin standard sample 0.03g (being accurate to 0.0002g) is weighed in 50mL volumetric flasks, with 70% first
Alcohol solution dissolves and is diluted to scale, sonic oscillation 5min, removes recovery to room temperature, standby.
(3) preparation of sample solution
2.0% efficient chlorine fluorine cyanogen aqueous suspension agent 0.03g sample (being accurate to 0.0002g) is weighed in 50mL volumetric flasks,
3g anhydrous sodium sulfates, then accurate addition cosolvent are added, it is rear accurately to add the dissolving of 70% methanol aqueous solution, wherein cosolvent：
70% methanol aqueous solution is 1:7, sonic oscillation 5min, recovery is removed to room temperature, has millipore filter filtering, filtrate through 0.45 μm
It is to be measured.
(4) chromatographiccondition
Chromatographic column：250mm × 6.5mm, 5 μm, WandaSilC18 posts；25 ± 1 DEG C of column temperature；Mobile phase：Methanol：Acetonitrile：Water
(V 30:40:30), flow velocity 1.0ml/min；Detection wavelength 235nm；Sampling volume： 10μl.
Wherein contrast experiment is tested with being not added with cosolvent, and testing result is as follows：Table 4 (does not add cosolvent)；Table 5
(addition cosolvent)；
The gamma cyhalothrin aqueous suspension agent assay method accuracy test of table 4
The gamma cyhalothrin aqueous suspension agent assay method accuracy test of table 5
From embodiment 1 and the testing result of embodiment 2, found out by above-mentioned testing result, after adding cosolvent, efficient chlorine
The degree of accuracy rate of recovery of flucythrinate aqueous suspension agent and aqueous emulsion increases substantially compared with contrast experiment；And the solution is just
Phase liquid chromatographic detection pyrethrin pesticide aqueous emulsion and aqueous suspension agent and the immiscible method of solvent, wherein cosolvent have safety
Property, feasibility, validity, and preparation method is simple to operation, when detecting pyrethrin pesticide aqueous emulsion and aqueous suspension agent, uses
It is convenient, on stability of drug products without influence, pyrethrin pesticide aqueous emulsion and aqueous suspension agent is mixed with solvent, can in detection
Rate of recovery during effectively improving the degree of accuracy, testing result is met Theoretical Prediction numerical value, reach the needs of detection.
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (4)
1. a kind of solution positive liquid chromatographic detection pyrethrin pesticide aqueous emulsion and aqueous suspension agent and the immiscible method of solvent, its
It is characterised by：A kind of cosolvent is added in detection method, co-solvent components include：Ethylenediamine, salicylic acid, glycine, 70% first
Alcohol solution.
2. solution positive liquid chromatographic detection pyrethrin pesticide aqueous emulsion according to claim 1 and aqueous suspension agent and solvent
Immiscible method, it is characterised in that：Wherein described ethylenediamine, salicylic acid, glycine, ethylenediamine：Salicylic acid：Glycine according to
0.1:1:0.5~0.5:1.0:0.8 carries out being configured to cosolvent basal liquid.
3. solution positive liquid chromatographic detection pyrethrin pesticide aqueous emulsion according to claim 2 and aqueous suspension agent and solvent
Immiscible method, it is characterised in that：70% methanol aqueous solution is added in basal liquid, wherein 70% methanol aqueous solution：Basal liquid
=7:3.
4. solution positive liquid chromatographic detection pyrethrin pesticide aqueous emulsion according to claim 3 and aqueous suspension agent and solvent
Immiscible method, it is characterised in that：Cosolvent preparation method is as follows：
(1) by ethylenediamine：Salicylic acid：Glycine is according to 0.1:1.0:0.2~0.5:1.0:0.6 ratio precision weighing, by second two
Amine, salicylic acid are placed in precision weighing in glass beaker, three after exact value decimal point；Glycine is placed on pan paper again accurate
Weigh, after the glycine of weighing is placed in ethylenediamine, salicylic acid is placed in glass beaker；
(2) first step 1 beaker is placed on heating magnetic stirring apparatus in ventilating kitchen, slow heating is warming up to 40 DEG C, and 200-
600rpm/min is stirred, and is well mixed；
(3) by 70% methanol aqueous solution with no more than 70% methanol aqueous solution after：Basal liquid (V7:3) ratio, step 2 is added
In mixed liquor, continue to heat 200-600rpm/min stirrings, until mixture is completely dissolved；
(4) step 3 mixed liquor is added in volumetric flask, 70% methanol aqueous solution is added in backward volumetric flask, until 70% methanol
The aqueous solution：Basal liquid (V7:3)；
(5) solution bottle,suction after step 4 constant volume and 0.45 μm of organic filter membrane are filtered 2 times, pressure 0.1Mpa, removes mixed liquor
Middle impurity；
(6) solution after suction filtration is fitted into after totally sterilizing in blue mouth bottle, bottle cap is not easy to tighten, and bottle cap easily covers；
(7) blue lid bottle of the step 6 equipped with mixed liquor is placed in ultrasonic 5-15min in ultrafilter after, ultrasound terminate after by blue lid bottle
Tighten and be positioned over 0-4 DEG C of reagent storage refrigerator.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101019530A (en) * | 2007-03-15 | 2007-08-22 | 周本新 | Azacycle containing pesticide microemulsion and its prepn |
| CN101554159A (en) * | 2008-04-11 | 2009-10-14 | 北京绿色农华生物工程技术有限公司 | Fenpropathrin microemulsion and preparation method thereof |
| CN101690712A (en) * | 2009-08-25 | 2010-04-07 | 武汉武药科技有限公司 | Sitafloxacin eye drop and preparation method thereof |
| CN101726589A (en) * | 2009-11-20 | 2010-06-09 | 江南大学 | Method for preparing group selectivity immunity affinity chromatographic column of synthetic pyrethroid medicaments |
-
2017
- 2017-09-30 CN CN201710919119.2A patent/CN107843659A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101019530A (en) * | 2007-03-15 | 2007-08-22 | 周本新 | Azacycle containing pesticide microemulsion and its prepn |
| CN101554159A (en) * | 2008-04-11 | 2009-10-14 | 北京绿色农华生物工程技术有限公司 | Fenpropathrin microemulsion and preparation method thereof |
| CN101690712A (en) * | 2009-08-25 | 2010-04-07 | 武汉武药科技有限公司 | Sitafloxacin eye drop and preparation method thereof |
| CN101726589A (en) * | 2009-11-20 | 2010-06-09 | 江南大学 | Method for preparing group selectivity immunity affinity chromatographic column of synthetic pyrethroid medicaments |
Non-Patent Citations (2)
| Title |
|---|
| DENISE ZUCCARI BISSACOT 等: "HPLC Determination of Flumethrin, Deltamethrin, Cypermethrin, and Cyhalothrin Residues in the Milk and Blood of Lactating Dairy Cows", 《JOURNAL OF ANALYTICAL TOXICOLOGY》 * |
| 宋健荣 等: "氯氟氰菊酯水乳剂的液相色谱分析", 《农药科学与管理》 * |
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Application publication date: 20180327 |