CN100487449C - High performance liquid chromatography analysis method for azadirachtin in water-based pesticide preparation - Google Patents
High performance liquid chromatography analysis method for azadirachtin in water-based pesticide preparation Download PDFInfo
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- CN100487449C CN100487449C CNB2005100487600A CN200510048760A CN100487449C CN 100487449 C CN100487449 C CN 100487449C CN B2005100487600 A CNB2005100487600 A CN B2005100487600A CN 200510048760 A CN200510048760 A CN 200510048760A CN 100487449 C CN100487449 C CN 100487449C
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Abstract
The invention discloses a high-effective gas-chromatography analysis method of melicitrin in the pesticide water fundamental mode agent, which is characterized by the following: adapting liquid-liquid allocation method to purify the water fundamental mode agent sample; taking the organic solvent or water as flow phase to make high effective gas-chromatography column of different polarities; utilizing ultraviolet detector or diode array detector to do gas-chromatography quantitative analysis of melicitrin in the pesticide water fundamental mode agent.
Description
Technical field
The present invention relates to the HPLC analytical method of nimbin in the water-based pesticide type preparation, its technical field belongs to analysis of agricultural drugs method.
Background technology
Nimbin is a kind of vegetable source pesticide active component that extracts from neem kernel, and various insects is had good insecticidal activity.The mechanism of action of nimbin is to make insect antifeedant, avoid and keep away and suppress growing of insect, and most of insects are had repelling and killing efficacy, and nontoxic to warm-blooded animal, and insect is developed immunity to drugs, and the long characteristics of tool efficiency time.Can be used for preventing and treating 200 more and to plant farming, woods, storage and sanitary insect pest, especially insects such as Lepidoptera, coleoptera and Diptera are had special efficacy, be the wide spectrum of generally acknowledging in the world, efficient, low toxicity, easily degrade, the novel pesticide of environmental friendliness of noresidue.The pesticidal preparations that contains nimbin at present is based on missible oil.The aqua type preparation of nimbin is compared with missible oil, and have that production cost is low, Environmental compatibility good, meet non-polluted farm product and produce advantages such as agricultural chemicals operating specification, be the future thrust of nimbin pesticidal preparations.About the preparation and the application of nimbin aqua type preparation, the existing report of relevant scientific and technical literature.Because the auxiliary agent in the aqua type preparation is more, the composition more complicated of whole system, if adopt common direct sample to analyze, impurity can produce serious disturbance to the mensuration of effective constituent.Relevant can effectively the impurity in the aqua type preparation being removed carried out the analytical approach of nimbin in the aqua type preparation, up to the present still do not have report.
Summary of the invention
The invention provides the HPLC analytical method of nimbin in a kind of water-based pesticide type preparation, have easy, accurate, quick, reliable characteristics, the quantitative test to effective constituent nimbin in the water-based pesticide type preparation has important practical value.
The present invention is achieved in that
1. the preparation of standard solution
Take by weighing 50～2000mg nimbin standard specimen in volumetric flask, with constant volume behind the organic solvent dissolution;
2. the preparation of sample pretreatment and sample solution
Take by weighing contain be equivalent to nimbin effective constituent in the standard solution nimbin aqua type preparation in volumetric flask, add and identical organic solvent and the water of standard solution preparation volumetric flask volume, the ratio of organic solvent and water is 1: 1～10, supersonic oscillations extractions 1～10min, leave standstill or centrifugal layering after take out organic phase and filter.Pipette the organic phase evaporate to dryness in container after 5～50mL filters, add organic solvent 5～50mL 1～10min that on ultrasonic oscillator, strips, go in the volume volumetric flask long-pending identical and use the organic solvent constant volume with pipetting liquid, to be measured after the filtration.
3. measure
The testing sample of step (2) being used the performance liquid chromatographic column of opposed polarity, make moving phase with the mixing material of organic solvent or water or organic solvent and water, is 10～50 ℃ at post oven temperature, degree; Flow rate of mobile phase is 0.1～10mL/min; Detecting wavelength is under the chromatographic condition of 190～900nm, adopts UV-detector or diode array detector, and nimbin is carried out the high performance liquid chromatography quantitative test.
Aqua type preparation described in the present invention is a kind of in aqua, aqueous emulsion, microemulsion, emulsifiable concentrate, aqueous suspension agent, colloidal suspending agent, suspension concentrates and the soluble liquid.
Organic solvent described in the present invention is one or more mixing in methylene chloride, methenyl choloride, ethyl acetate, toluene, dimethylbenzene, methyl alcohol, acetonitrile, ether, hexane, normal hexane, the cyclohexane.
The performance liquid chromatographic column of the opposed polarity described in the present invention is silicagel column, C
8Post or C
18Post.
Described detection wavelength is 190～210nm or 220～900nm.
UV-detector described in the present invention is that fixed wave length is that UV-detector or the variable range of wavelengths of 254nm is the UV-detector of 190～900nm.
The pesticidal preparations that contains nimbin at present is based on missible oil, and the aqua type preparation is compared with missible oil, and have that production cost is low, Environmental compatibility good, meet non-polluted farm product and produce advantages such as agricultural chemicals operating specification, be the future thrust of nimbin pesticidal preparations.About the preparation and the application of nimbin aqua type preparation, the existing report of relevant scientific and technical literature.Because the auxiliary agent in the aqua type preparation is more, the composition more complicated of whole system, if adopt common direct sample to analyze, impurity can produce serious disturbance to the mensuration of effective constituent.The method that the present invention adopts is after interference impurity is removed, effective constituent to be measured again, can be accurately, quickly and reliably to the quantitative test of nimbin in the aqua type preparation.Up to the present the HPLC analytical method of nimbin in this aqua type preparation does not still have report.The effectively foundation of the HPLC analytical method of nimbin in the aqua type preparation, to accurately, quickly and reliably to the quantitative test of nimbin in the aqua type preparation with expand the application of nimbin aqua type preparation in agricultural production practice, significant.
Embodiment
Embodiment one
1. the preparation of standard solution
Take by weighing 50mg nimbin standard specimen in the 25mL volumetric flask, with dissolve with methanol and be settled to scale, the organic membrane filtration of 0.45um.
2. the preparation of sample pretreatment and sample solution
Take by weighing contain 50mg nimbin effective constituent nimbin aqua type preparation in the 25mL volumetric flask, the mixing material that adds 25mL organic solvent and water, the ratio of organic solvent and water is 1: 1, supersonic oscillations extractions 1min, leave standstill or centrifugal layering after take out organic phase and filter.Pipette the organic phase evaporate to dryness in container after 5mL filters, add the organic solvent 5mL 1min that on ultrasonic oscillator, strips, go to volume and amass in the identical volumetric flask and use the organic solvent constant volume with pipetting liquid, to be measured behind the organic membrane filtration of 0.45um.
3. measure
The testing sample of step 2 is used the C of 150mm * 4.0mm (i.d)
18Performance liquid chromatographic column with volume ratio is: water: the mixing material of acetonitrile=56: 44 is made moving phase, is 10 ℃ at post oven temperature, degree; Flow rate of mobile phase is 0.1mL/min; Detecting wavelength is under the chromatographic condition of 190nm, adopts UV-detector that nimbin is carried out the high performance liquid chromatography quantitative test.
Embodiment two
1. the preparation of standard solution
Take by weighing 100mg nimbin standard specimen in the 25mL volumetric flask, with dissolve with methanol and be settled to scale, the organic membrane filtration of 0.45um.
2. the preparation of sample pretreatment and sample solution
Take by weighing contain 100mg nimbin effective constituent nimbin aqua type preparation in the 25mL volumetric flask, the mixing material that adds 25mL organic solvent and water, the ratio of organic solvent and water is 1: 5, supersonic oscillations extractions 5min, leave standstill or centrifugal layering after take out organic phase and filter.Pipette the organic phase evaporate to dryness in container after 10mL filters, add the organic solvent 10mL 5min that on ultrasonic oscillator, strips, go to volume and amass in the identical volumetric flask and use the organic solvent constant volume with pipetting liquid, to be measured behind the organic membrane filtration of 0.45um.
3. measure
The testing sample of step 2 is used the C of 150mm * 4.0mm (i.d)
18Performance liquid chromatographic column with volume ratio is: water: the mixing material of acetonitrile=56: 44 is made moving phase, is 10 ℃ at post oven temperature, degree; Flow rate of mobile phase is 1.0mL/min; Detecting wavelength is under the chromatographic condition of 218nm, adopts UV-detector that nimbin is carried out the high performance liquid chromatography quantitative test.
Embodiment three
1. the preparation of standard solution
Take by weighing 2000mg nimbin standard specimen in the 50mL volumetric flask, with dissolve with methanol and be settled to scale, the organic membrane filtration of 0.45um.
2. the preparation of sample pretreatment and sample solution
Take by weighing contain 2000mg nimbin effective constituent nimbin aqua type preparation in the 50mL volumetric flask, the mixing material that adds 50mL organic solvent and water, the ratio of organic solvent and water is 1: 10, supersonic oscillations extractions 10min, leave standstill or centrifugal layering after take out organic phase and filter.Pipette the organic phase evaporate to dryness in container after 50mL filters, add the organic solvent 50mL 10min that on ultrasonic oscillator, strips, go to volume and amass in the identical volumetric flask and use the organic solvent constant volume with pipetting liquid, to be measured behind the organic membrane filtration of 0.45um.
3. measure
The testing sample of step 2 is used the C of 150mm * 4.0mm (i.d)
18Performance liquid chromatographic column with volume ratio is: water: the mixing material of acetonitrile=56: 44 is made moving phase, is 50 ℃ at post oven temperature, degree; Flow rate of mobile phase is 10mL/min; Detecting wavelength is under the chromatographic condition of 900nm, adopts UV-detector that nimbin is carried out the high performance liquid chromatography quantitative test.
Embodiment four
1. the preparation of standard solution
Take by weighing 50mg nimbin standard specimen in the 25mL volumetric flask, with dissolve with methanol and be settled to scale, the organic membrane filtration of 0.45um.
2. the preparation of sample pretreatment and sample solution
Take by weighing contain 50mg nimbin effective constituent nimbin aqua type preparation in the 25mL volumetric flask, the mixing material that adds 25mL organic solvent and water, the ratio of organic solvent and water is 1: 1, supersonic oscillations extractions 1min, leave standstill or centrifugal layering after take out organic phase and filter.Pipette the organic phase evaporate to dryness in container after 5mL filters, add the organic solvent 5mL 1min that on ultrasonic oscillator, strips, go to volume and amass in the identical volumetric flask and use the organic solvent constant volume with pipetting liquid, to be measured behind the organic membrane filtration of 0.45um.
3. measure
The testing sample of step 2 is used the C of 150mm * 4.0mm (i.d)
18Performance liquid chromatographic column with volume ratio is: water: the mixing material of acetonitrile=56: 44 is made moving phase, is 10 ℃ at post oven temperature, degree; Flow rate of mobile phase is 0.1mL/min; Detecting wavelength is under the chromatographic condition of 190nm, adopts diode array detector that nimbin is carried out the high performance liquid chromatography quantitative test.
Embodiment five
1. the preparation of standard solution
Take by weighing 100mg nimbin standard specimen in the 25mL volumetric flask, with dissolve with methanol and be settled to scale, the organic membrane filtration of 0.45um.
2. the preparation of sample pretreatment and sample solution
Take by weighing contain 100mg nimbin effective constituent nimbin aqua type preparation in the 25mL volumetric flask, the mixing material that adds 25mL organic solvent and water, the ratio of organic solvent and water is 1: 5, supersonic oscillations extractions 5min, leave standstill or centrifugal layering after take out organic phase and filter.Pipette the organic phase evaporate to dryness in container after 10mL filters, add the organic solvent 10mL 5min that on ultrasonic oscillator, strips, go to volume and amass in the identical volumetric flask and use the organic solvent constant volume with pipetting liquid, to be measured behind the organic membrane filtration of 0.45um.
3. measure
The testing sample of step 2 is used the C of 150mm * 4.0mm (i.d)
18Performance liquid chromatographic column with volume ratio is: water: the mixing material of acetonitrile=56: 44 is made moving phase, is 10 ℃ at post oven temperature, degree; Flow rate of mobile phase is 1.0mL/min; Detecting wavelength is under the chromatographic condition of 218nm, adopts diode array detector that nimbin is carried out the high performance liquid chromatography quantitative test.
Embodiment six
1. the preparation of standard solution
Take by weighing 2000mg nimbin standard specimen in the 50mL volumetric flask, with dissolve with methanol and be settled to scale, the organic membrane filtration of 0.45um.
2. the preparation of sample pretreatment and sample solution
Take by weighing contain 2000mg nimbin effective constituent nimbin aqua type preparation in the 50mL volumetric flask, the mixing material that adds 50mL organic solvent and water, the ratio of organic solvent and water is 1: 10, supersonic oscillations extractions 10min, leave standstill or centrifugal layering after take out organic phase and filter.Pipette the organic phase evaporate to dryness in container after 50mL filters, add the organic solvent 50mL 10min that on ultrasonic oscillator, strips, go to volume and amass in the identical volumetric flask and use the organic solvent constant volume with pipetting liquid, to be measured behind the organic membrane filtration of 0.45um.
3. measure
The testing sample of step 2 is used the C of 150mm * 4.0mm (i.d)
18Performance liquid chromatographic column with volume ratio is: water: the mixing material of acetonitrile=56: 44 is made moving phase, is 50 ℃ at post oven temperature, degree; Flow rate of mobile phase is 10mL/min; Detecting wavelength is under the chromatographic condition of 900nm, adopts diode array detector that nimbin is carried out the high performance liquid chromatography quantitative test.
Claims (5)
1. the HPLC analytical method of nimbin in the water-based pesticide type preparation the steps include:
(1) preparation of standard solution
Take by weighing 50～2000mg nimbin standard specimen in volumetric flask, with constant volume behind the dissolve with methanol;
(2) preparation of sample pretreatment and sample solution
Take by weighing contain be equivalent to nimbin effective constituent in the standard solution nimbin aqua type preparation in volumetric flask, add and identical organic solvent and the water of standard solution preparation volumetric flask volume, the ratio of organic solvent and water is 1: 1～10, supersonic oscillations extraction 1～10min, leave standstill or centrifugal layering after take out organic phase and filter, pipette the organic phase evaporate to dryness in container after 5～50mL filters, add organic solvent 5～50mL 1～10min that on ultrasonic oscillator, strips, go in the volume volumetric flask long-pending identical and use the organic solvent constant volume with pipetting liquid, to be measured after filtering;
Described organic solvent is one or more mixing in methylene chloride, methenyl choloride, ethyl acetate, toluene, dimethylbenzene, methyl alcohol, acetonitrile, ether, the hexane;
(3) measure
The testing sample of step (2) is used the performance liquid chromatographic column of opposed polarity, with volume ratio be: water: the mixing material of acetonitrile=56: 44 is made moving phase, is 10～50 ℃ at post oven temperature, degree; Flow rate of mobile phase is 0.1～10mL/min; Detecting wavelength is under the chromatographic condition of 190～900nm, adopts UV-detector or diode array detector, and nimbin is carried out the high performance liquid chromatography quantitative test;
The performance liquid chromatographic column of described opposed polarity is silicagel column or C
8Post or C
18Post.
2. the HPLC analytical method of nimbin in the water-based pesticide type preparation according to claim 1 is characterized in that: described aqua type preparation is a kind of in aqua, aqueous emulsion, microemulsion, emulsifiable concentrate, aqueous suspension agent, colloidal suspending agent, suspension concentrates and the soluble liquid.
3. the HPLC analytical method of nimbin in the water-based pesticide type preparation according to claim 1, it is characterized in that: described detection wavelength is 190～210nm.
4. the HPLC analytical method of nimbin in the water-based pesticide type preparation according to claim 1, it is characterized in that: described detection wavelength is 220～900nm.
5. the HPLC analytical method of nimbin in the water-based pesticide type preparation according to claim 1 is characterized in that: described UV-detector is that fixed wave length is that UV-detector or the variable range of wavelengths of 254nm is the UV-detector of 190～900nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100487600A CN100487449C (en) | 2005-12-27 | 2005-12-27 | High performance liquid chromatography analysis method for azadirachtin in water-based pesticide preparation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100487600A CN100487449C (en) | 2005-12-27 | 2005-12-27 | High performance liquid chromatography analysis method for azadirachtin in water-based pesticide preparation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1790010A CN1790010A (en) | 2006-06-21 |
| CN100487449C true CN100487449C (en) | 2009-05-13 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100487600A Expired - Fee Related CN100487449C (en) | 2005-12-27 | 2005-12-27 | High performance liquid chromatography analysis method for azadirachtin in water-based pesticide preparation |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103450227B (en) * | 2013-08-30 | 2015-12-09 | 中国科学院昆明植物研究所 | The print former medicine of chinaberry and containing its sterilant and its preparation method and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2184564A1 (en) * | 1995-08-31 | 1997-03-01 | Bhagavathula Ravindranath | Chromatographic method and its use for separation of azadirachtin |
| CN1362020A (en) * | 2001-12-27 | 2002-08-07 | 海南英得利生物技术开发有限公司 | Nim mextractive producing process |
-
2005
- 2005-12-27 CN CNB2005100487600A patent/CN100487449C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2184564A1 (en) * | 1995-08-31 | 1997-03-01 | Bhagavathula Ravindranath | Chromatographic method and its use for separation of azadirachtin |
| CN1362020A (en) * | 2001-12-27 | 2002-08-07 | 海南英得利生物技术开发有限公司 | Nim mextractive producing process |
Non-Patent Citations (4)
| Title |
|---|
| 0.3%印楝素乳油的高效液相色谱方法. 何道航等.农药，第40卷第9期. 2001 |
| 0.3%印楝素乳油的高效液相色谱方法. 何道航等.农药，第40卷第9期. 2001 * |
| 印楝种仁中印楝素含量的快速液相色谱分析. 宗乾收等.农药，第42卷第4期. 2003 |
| 印楝种仁中印楝素含量的快速液相色谱分析. 宗乾收等.农药，第42卷第4期. 2003 * |
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Granted publication date: 20090513 Termination date: 20121227 |