CN110146630A - A kind of method of the effective content of muscalure in detection Pesticidal composition - Google Patents
A kind of method of the effective content of muscalure in detection Pesticidal composition Download PDFInfo
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- CN110146630A CN110146630A CN201910552767.8A CN201910552767A CN110146630A CN 110146630 A CN110146630 A CN 110146630A CN 201910552767 A CN201910552767 A CN 201910552767A CN 110146630 A CN110146630 A CN 110146630A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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Abstract
Belong to analysis of agricultural drugs technical field the invention belongs to bright, and in particular to a method of the effective content of muscalure in detection Pesticidal composition.The following steps are included: 1) selection of solvent；2) preparation of sample solution: being added muscalure, methanol dissolution in volumetric flask, and constant volume shakes up；3) preparation of standard specimen solution: being separately added into the muscalure of various concentration, methylene chloride dissolution in volumetric flask, and constant volume simultaneously shakes up；4) it draws standard curve: being analyzed using the standard specimen solution that gas chromatography-mass spectrography prepares step 3), using concentration as abscissa, peak area is that ordinate draws standard curve；5) sample solution is detected: sample solution is analyzed using gas chromatography-mass spectrography, obtains peak area, peak area substituted into the regression equation of standard curve, obtain the effective content of muscalure in sample.This method can efficiently separate isomers and the content detected containing low content muscalure in mixture accurate and reliable, that reproducibility is high.
Description
Technical field
The invention belongs to bright belong to analysis of agricultural drugs technical field, and in particular to there is muscalure in a kind of detection Pesticidal composition
The method for imitating content.
Background technique
Muscalure (Cis-9-Tricosene) also known as attractant, molecular formula are C23H46, molecular weight 322.6113,
CAS registration number is 27519-02-4, one of agricultural chemicals.The entitled cis- 9- tricosene of muscalure chemistry, be initially by
Carlson et al. is isolated out of female housefly body, after by mountain pass scholar company, Switzerland development and production.Since muscalure has to people
Raise that toxicity is low, use scope is wide, at the same have the advantages that it is low in usage amount, to make it a kind of important insect attractant
Agent.
Muscalure is trapped and killed there are two types of the uses generally of mode, a kind of to mate as gyplure interference insect；Another is lured
Worm alkene can be mixed with poisonous substance, trap insect's food-taking to trap and kill.
Currently, being commonly used in mixed way in the market with toxic agent, such as muscalure-DDVP mixture, muscalure Methomyl is mixed
Agent etc., significant effect.Since usage amount of the muscalure with isomers and in mixture is very low (6 ‰ -0.8%), to increase
Detection difficulty.And using the muscalure mixture of GC-MS (gas chromatography-mass spectrum) quantitative detection low concentration, there is not been reported.
Summary of the invention
In order to overcome the shortcomings in the prior art, the present invention provides a kind of effective content for detecting muscalure in Pesticidal composition
Method；This method can efficiently separate isomers and accurate and reliable, reproducibility it is high detect to lure in mixture containing low content
The content of worm alkene.
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of method of the effective content of muscalure in detection Pesticidal composition, comprising the following steps:
1) preparation of sample solution: being added muscalure, methanol dissolution in volumetric flask, and constant volume shakes up；
2) muscalure of various concentration, methylene chloride dissolution, constant volume the preparation of standard specimen solution: are separately added into volumetric flask
And it shakes up；Be conducive to standard liquid preservation using methylene chloride but be detrimental to sample dissolution, so sample is dissolved using methanol；
3) it draws standard curve: being analyzed using the standard specimen solution that gas chromatography-mass spectrography prepares step 2), with
Concentration is abscissa, and peak area is that ordinate draws standard curve；
4) sample solution is detected: sample solution is analyzed using gas chromatography-mass spectrography, obtains peak face
Peak area is substituted into the regression equation of standard curve, obtains the effective content of muscalure in sample by product.
As a preferred solution of the present invention, the specific steps of the preparation of the standard specimen solution in the step 2) are as follows: weigh and lure
Into 100.0ml volumetric flask, methylene chloride dissolution, constant volume simultaneously shakes up worm alkene standard specimen 53.6mg；0.01,0.1 is accurately pipetted respectively,
Into 100.0ml volumetric flask, methylene chloride dissolution, constant volume simultaneously shakes up 0.5,0.8,1.0,1.5 and 2.0ml.
As a preferred solution of the present invention, chromatographic condition in gas-chromatography in the gas chromatography-mass spectrography are as follows: sample introduction
140~300 DEG C of mouth, carrier gas is helium, 0.5~1.0ml/min of flow velocity, split ratio 20:1,0.5~1.0 μ l of sampling volume, post case
60 DEG C, 5min is kept, 280 DEG C is risen to 5 DEG C/min, keeps 5min.
As a preferred solution of the present invention, Mass Spectrometry Conditions in the gas chromatography-mass spectrography are as follows: electron bombardment ionization source EI,
Electron bombardment voltage 70eV, 250 DEG C of transmission line, 230 DEG C of ion source temperature, 150 DEG C of level four bars temperature, solvent delay 4min is swept
Retouch Mode S IM, quota ion 83, qualitative ion 55,69,97,111.
As a preferred solution of the present invention, the chromatographic column in the gas chromatography-mass spectrography in gas-chromatography selects HP-
5MS type capillary chromatographic column or other equivalent chromatographic columns.
Compared with prior art, the invention has the following advantages:
(1) this method simplicity, good separating effect, accurate, favorable reproducibility, can be used for the quantitative detection of muscalure mixture；
(2) this method test scope can also can be used for the trace of muscalure in mixture down to 0.0006% and high sensitivity
Detection；
(3) the dissolution influence and the selection of standard sample stock solution this method provides the selection of solvent for WDG dosage form.
Detailed description of the invention
Fig. 1 is the resulting muscalure chromatogram of embodiment 1；
Fig. 2 is the resulting muscalure mass spectrogram of embodiment 1；
Fig. 3 is the resulting muscalure canonical plotting of embodiment 1.
Specific embodiment
Below by specific embodiment, invention is further described in detail.But those skilled in the art will manage
Solution, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.Specific skill is not specified in embodiment
Art or condition person, described technology or conditions carry out to specifications according to the literature in the art.Agents useful for same or instrument
Production firm person is not specified, being can be with conventional products that are commercially available.
Pesticide trapping mixture sample in embodiment is commercially available gained, and the pesticide traps and kills mixture sample muscalure content mark
Indicating value is 0.025% (± 0.005%).
Embodiment 1
A kind of method of the effective content of muscalure in detection Pesticidal composition, comprising the following steps:
1) preparation of sample solution: being added muscalure, methanol dissolution in volumetric flask, and constant volume shakes up；
2) muscalure of various concentration, methylene chloride dissolution, constant volume the preparation of standard specimen solution: are separately added into volumetric flask
And it shakes up；Be conducive to standard liquid preservation using methylene chloride but be detrimental to sample dissolution, so sample is dissolved using methanol；
3) it draws standard curve: being analyzed using the standard specimen solution that gas chromatography-mass spectrography prepares step 2), with
Concentration is abscissa, and peak area is that ordinate draws standard curve；
4) sample solution is detected: sample solution is analyzed using gas chromatography-mass spectrography, obtains peak face
Peak area is substituted into the regression equation of standard curve, obtains the effective content of muscalure in sample by product.
Wherein, the specific steps of the preparation of the standard specimen solution in the step 2) are as follows: weigh muscalure standard specimen 53.6mg extremely
In 100.0ml volumetric flask, methylene chloride dissolution, constant volume is simultaneously shaken up；0.01,0.1,0.5,0.8,1.0,1.5 is accurately pipetted respectively
With 2.0ml into 100.0ml volumetric flask, methylene chloride dissolution, constant volume is simultaneously shaken up.
Chromatographic condition in gas-chromatography in the gas chromatography-mass spectrography are as follows: 140 DEG C of injection port, carrier gas is helium, stream
Fast 0.5ml/min, split ratio 20:1,0.5 μ l of sampling volume, keep 5min by 60 DEG C of post case, rise to 280 DEG C with 5 DEG C/min, protect
Hold 5min.
Mass Spectrometry Conditions in the gas chromatography-mass spectrography are as follows: electron bombardment ionization source EI, electron bombardment voltage 70eV, transmission
250 DEG C of line, 230 DEG C of ion source temperature, 150 DEG C of level four bars temperature, solvent delay 4min, scan pattern SIM, quota ion 83,
Qualitative ion 55,69,97,111.
In the gas chromatography-mass spectrography in gas-chromatography chromatographic column selection HP-5MS type capillary chromatographic column etc.
Imitate chromatographic column.
Embodiment 2
A kind of method of the effective content of muscalure in detection Pesticidal composition, comprising the following steps:
1) preparation of sample solution: being added muscalure, methanol dissolution in volumetric flask, and constant volume shakes up；
2) muscalure of various concentration, methylene chloride dissolution, constant volume the preparation of standard specimen solution: are separately added into volumetric flask
And it shakes up；Be conducive to standard liquid preservation using methylene chloride but be detrimental to sample dissolution, so sample is dissolved using methanol；
3) it draws standard curve: being analyzed using the standard specimen solution that gas chromatography-mass spectrography prepares step 2), with
Concentration is abscissa, and peak area is that ordinate draws standard curve；
4) sample solution is detected: sample solution is analyzed using gas chromatography-mass spectrography, obtains peak face
Peak area is substituted into the regression equation of standard curve, obtains the effective content of muscalure in sample by product.
As a preferred solution of the present invention, the specific steps of the preparation of the standard specimen solution in the step 2) are as follows: weigh and lure
Into 100.0ml volumetric flask, methylene chloride dissolution, constant volume simultaneously shakes up worm alkene standard specimen 53.6mg；0.01,0.1 is accurately pipetted respectively,
Into 100.0ml volumetric flask, methylene chloride dissolution, constant volume simultaneously shakes up 0.5,0.8,1.0,1.5 and 2.0ml.
Wherein, chromatographic condition in gas-chromatography in the gas chromatography-mass spectrography are as follows: 140~300 DEG C of injection port, carry
Gas is helium, flow velocity 1.0ml/min, split ratio 20:1, and 1.0 μ l of sampling volume, keeps 5min, with 5 DEG C/min liter by 60 DEG C of post case
To 280 DEG C, 5min is kept.
Mass Spectrometry Conditions in the gas chromatography-mass spectrography are as follows: electron bombardment ionization source EI, electron bombardment voltage 70eV, transmission
250 DEG C of line, 230 DEG C of ion source temperature, 150 DEG C of level four bars temperature, solvent delay 4min, scan pattern SIM, quota ion 83,
Qualitative ion 55,69,97,111.
Chromatographic column in the gas chromatography-mass spectrography in gas-chromatography selects HP-5MS type capillary chromatographic column.
Embodiment 3
A kind of method of the effective content of muscalure in detection Pesticidal composition, comprising the following steps:
Chromatographic condition in gas-chromatography in gas chromatography-mass spectrography are as follows: 280 DEG C of injection port, carrier gas (high-purity helium), stream
Fast 1.0ml/min, split ratio 20:1,1.0 μ l of sampling volume, keep 5min by 60 DEG C of post case, rise to 280 DEG C with 5 DEG C/min, protect
Hold 5min；Chromatographic column: HP-5MS (30m × 0.25mm × 0.25 μm)
Mass Spectrometry Conditions in gas chromatography-mass spectrography are as follows: electron bombardment ionization source (EI), 70eV, 250 DEG C of transmission line, ion source
230 DEG C, 150 DEG C of level four bars, solvent delay 4min, scan pattern SIM, quota ion 83, qualitative ion 55,69,97,111.
Chromatographic column in gas chromatography-mass spectrography in gas-chromatography selects HP-5MS type capillary chromatographic column.
It is to accurately weigh muscalure standard specimen 53.6mg referring to product using the muscalure that Dr.Ehrenstorfer GmbH is provided
Into 100.0ml volumetric flask, methylene chloride dissolution, constant volume is simultaneously shaken up.0.01,0.1,0.5 is accurately pipetted with pipette respectively,
0.8,1.0,1.5 and 2.0ml into 100.0ml volumetric flask, methylene chloride dissolution, constant volume and shake up this for standard curve series it is molten
Liquid.Equation of linear regression (as shown in Figure 3) is obtained into chromatography test (chromatographic results are as depicted in figs. 1 and 2).
Muscalure sample solution: the sample about 0.9g of certain company offer is accurately weighed into 100.0ml volumetric flask, methanol is molten
Solution, constant volume simultaneously shake up this as sample solution.
The experiment of the muscalure sample solution rate of recovery: it is accurate to claim sample about 0.9g into 100.0ml volumetric flask, table is accurately added
The quality of listed standard specimen in 1, methanol dissolution, constant volume simultaneously shake up this as mark-on test solution.
Calculation formula:
Rate of recovery calculation formula:
C1: standardized sample test concentrations；
C2: sample test concentration；
C3: scalar quantity
Sample concentration calculates:
As shown in Figure 3: using standard solution response as ordinate, prepared concentration of standard solution is that abscissa returns
Equation obtains y=731188x-27.644 (r2=0.9998).
Calculating contained muscalure in sample to obtain content according to linear equation is 0.030%, and the rate of recovery is 90~105%.It takes
Satisfactory result.
The rate of recovery of 1 method of table tests (n=3)
The above is only preferred embodiments of the present invention, is not intended to limit the scope of the present invention,
Therefore any trickle amendment, equivalent variations and modification made to the above embodiment according to the technical essence of the invention, belong to
In the range of technical solution of the present invention.
Claims (5)
1. a kind of method of the effective content of muscalure in detection Pesticidal composition, which comprises the following steps:
1) preparation of sample solution: being added muscalure, methanol dissolution in volumetric flask, and constant volume shakes up；
2) preparation of standard specimen solution: being separately added into the muscalure of various concentration, methylene chloride dissolution in volumetric flask, and constant volume simultaneously shakes
It is even；
3) it draws standard curve: being analyzed using the standard specimen solution that gas chromatography-mass spectrography prepares step 2), with concentration
For abscissa, peak area is that ordinate draws standard curve；
4) sample solution is detected: sample solution is analyzed using gas chromatography-mass spectrography, obtains peak area,
Peak area is substituted into the regression equation of standard curve, obtains the effective content of muscalure in sample.
2. the method for the effective content of muscalure in a kind of detection Pesticidal composition according to claim 1, which is characterized in that
The specific steps of the preparation of standard specimen solution in the step 2) are as follows: weigh muscalure standard specimen 53.6mg to 100.0ml volumetric flask
In, methylene chloride dissolution, constant volume simultaneously shakes up；0.01,0.1,0.5,0.8,1.0,1.5 and 2.0ml is accurately pipetted respectively extremely
In 100.0ml volumetric flask, methylene chloride dissolution, constant volume is simultaneously shaken up.
3. the method for the effective content of muscalure in a kind of detection Pesticidal composition according to claim 1, which is characterized in that
Chromatographic condition in gas-chromatography in the gas chromatography-mass spectrography are as follows: 140~300 DEG C of injection port, carrier gas is helium, flow velocity
0.5~1.0ml/min, split ratio 20:1,0.5~1.0 μ l of sampling volume, are kept 5min, are risen to 5 DEG C/min by 60 DEG C of post case
280 DEG C, keep 5min.
4. the method for the effective content of muscalure in a kind of detection Pesticidal composition according to claim 1, which is characterized in that
Mass Spectrometry Conditions in the gas chromatography-mass spectrography are as follows: electron bombardment ionization source EI, electron bombardment voltage 70eV, 250 DEG C of transmission line,
230 DEG C of ion source temperature, 150 DEG C of level four bars temperature, solvent delay 4min, scan pattern SIM, quota ion 83, qualitative ion
55,69,97,111.
5. the method for the effective content of muscalure in a kind of detection Pesticidal composition according to claim 3, which is characterized in that
Chromatographic column selection HP-5MS type capillary chromatographic column or other equivalent colors in the gas chromatography-mass spectrography in gas-chromatography
Compose column.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112471167A (en) * | 2020-12-28 | 2021-03-12 | 镇江先锋植保科技有限公司 | Imidacloprid-containing water dispersible granule with trapping and killing capacity and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3932616A (en) * | 1972-06-26 | 1976-01-13 | Otto Meresz | Insect attractant composition |
| US20110293553A1 (en) * | 2010-05-28 | 2011-12-01 | Tai-Teh Wu | Identification of insect attractant, arresting, and/or aggregation compounds and methods thereof |
| CN109781912A (en) * | 2019-04-01 | 2019-05-21 | 中国测试技术研究院 | With the method for 29 kinds of auxiliary agent contents in Gas Chromatography-Mass Spectrometry pesticidal preparations |
-
2019
- 2019-06-25 CN CN201910552767.8A patent/CN110146630A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3932616A (en) * | 1972-06-26 | 1976-01-13 | Otto Meresz | Insect attractant composition |
| US20110293553A1 (en) * | 2010-05-28 | 2011-12-01 | Tai-Teh Wu | Identification of insect attractant, arresting, and/or aggregation compounds and methods thereof |
| CN109781912A (en) * | 2019-04-01 | 2019-05-21 | 中国测试技术研究院 | With the method for 29 kinds of auxiliary agent contents in Gas Chromatography-Mass Spectrometry pesticidal preparations |
Non-Patent Citations (2)
| Title |
|---|
| ERHAN,SZ 等: "Volatile by-products during heat polymerization of soybean oil", 《JOURNAL OF THE AMERICAN OIL CHEMISTS SOCIETY》 * |
| 付振方 等: "气相色谱-质谱联用法测定诱虫烯混剂中有效成分含量", 《现代农业科技》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112471167A (en) * | 2020-12-28 | 2021-03-12 | 镇江先锋植保科技有限公司 | Imidacloprid-containing water dispersible granule with trapping and killing capacity and preparation method thereof |
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Application publication date: 20190820 |