CN105301129B - Buprofezin and the method for Mobucin content in Buprofezin Mobucin compounding powder agent are determined simultaneously - Google Patents
Buprofezin and the method for Mobucin content in Buprofezin Mobucin compounding powder agent are determined simultaneously Download PDFInfo
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Abstract
The invention provides method that is a kind of while determining Buprofezin and Mobucin content in Buprofezin Mobucin compounding powder agent, is related to content of material detection technique field, this method is using filling C18The stainless steel column of bonded phase packings and the mobile phase progress sample component separation by phosphoric acid regulating ph value for 3 methanol+water, quantitatively detected using high performance liquid chromatograph and UV-detector and using peak area external standard method progress liquid chromatogram, it the method achieve Buprofezin in Buprofezin Mobucin compounding powder agent, two kinds of principle active components of Mobucin efficiently separate with each impurity composition, detected using with the UV-detector of liquid chromatograph, realize to the Buprofezin in compounding powder agent and Mobucin simultaneous quantitative, the assay method is simple to operate, analysis time is short, testing result is accurate.
Description
Technical field
It is more particularly to a kind of to determine Buprofezin-Mobucin compounding simultaneously the present invention relates to content of material detection technique field
Buprofezin and the method for Mobucin content in pulvis.
Background technology
Mobucin, Buprofezin are the preferable pesticide species for preventing and treating planthopper, and Mobucin single dose has quick-acting, less toxic
Feature, but the longevity of residure is short, needs application times more.Buprofezin single dose has the characteristics that efficient, less toxic, long-acting.Two kinds of single doses are passed through
Much time using all more or less generates the resistance to the action of a drug, and two kinds of single doses are compounded with certain proportion, can reach efficient, low
Malicious, quick-acting, long-acting preventing and treating planthopper, the effect of rice leafhopper.Detection for Mobucin-buprofezin compound pulvis, national standard
Temporarily without concrete regulation, in professional standard or company standard mostly using gas chromatogram fixative to the Mobucin in compounding powder agent,
Buprofezin content determines respectively（A kind of content of material in Mobucin, Buprofezin is first determined, then determines another material again
Content）, operation is relatively cumbersome, and analysis time is longer.Therefore, it is necessary to can be accurately quick while thiazine be detected by establishing one kind
Buprofezin, the detection method of two kinds of active ingredient of Mobucin in ketone Mobucin compounding powder agent, improve Buprofezin-Mobucin compounding
The quality testing efficiency of pulvis production, for Instructing manufacture.
The content of the invention
The technical problem to be solved in the present invention is to provide one kind can determine thiazine in Buprofezin-Mobucin compounding powder agent simultaneously
The method of the content of two kinds of active ingredient of ketone and Mobucin, the detection method analysis time is short, testing result is accurate.
In order to solve the above-mentioned technical problem, the present invention adopts the following technical scheme that：It is a kind of to determine Buprofezin-Mobucin simultaneously
Buprofezin and the method for Mobucin content in compounding powder agent, this method is using filling C18The stainless steel column of bonded phase packings and pass through
Phosphoric acid regulating ph value is that the mobile phase of 3 methanol+water carries out sample component separation, uses high performance liquid chromatograph and ultraviolet detection
Device simultaneously carries out liquid chromatogram using peak area external standard method and quantitatively detected, in the Buprofezin-Mobucin compounding powder agent Buprofezin with
The mass fraction of Mobucin is calculated as follows：
In above formula, A1--- in standard specimen solution, the average value of Buprofezin/Mobucin peak area；
A2--- in sample solution, the average value of Buprofezin/Mobucin peak area；
m1--- the quality of standard specimen, unit are gram（g）；
m2--- the quality of sample, unit are gram（g）；
W1--- the mass fraction of Buprofezin/Mobucin, numerical value are represented with percentage value in standard specimen.
Wherein, the stainless steel column column length 150-250mm, column internal diameter 0.46mm, the C18Bonded phase packings particle diameter is 5
μm。
The beneficial effect that the present invention obtains is：It is provided by the invention while determine in Buprofezin-Mobucin compounding powder agent
The method of Buprofezin and Mobucin content use Buprofezin in peak area external standard method parathiazine ketone-Mobucin compounding powder agent with it is different
Third prestige carries out liquid chromatogram and quantitatively detected, creatively selection filling C18The stainless steel column of bonded phase packings and adjusted by phosphoric acid
PH value be 3 methanol+water mobile phase carry out sample component separation, realize Buprofezin in Buprofezin-Mobucin compounding powder agent,
Two kinds of principle active components of Mobucin efficiently separate with each impurity composition, are examined using the UV-detector of liquid chromatograph
To survey, realize to the Buprofezin in compounding powder agent and Mobucin simultaneous quantitative, the assay method is simple to operate, analysis time is short,
Testing result is accurate.
Brief description of the drawings
Fig. 1 is using Buprofezin and Mobucin in detection method parathiazine ketone-Mobucin compounding powder agent provided by the invention
The liquid chromatogram for the specific detection example that content is measured；
Fig. 2 is using Buprofezin assay in detection method parathiazine ketone-Mobucin compounding powder agent provided by the invention
Linear relationship chart；
Fig. 3 is using Mobucin assay in detection method parathiazine ketone-Mobucin compounding powder agent provided by the invention
Linear relationship chart.
Embodiment
For the ease of the understanding of those skilled in the art, the present invention is made further with reference to specific embodiment
Bright, the content that embodiment refers to not is limitation of the invention.
Need to illustrate in advance, in detection method provided by the invention, the column length of stainless steel column can be in 150-
Selected between 250mm, final experimental result is simultaneously unaffected.Stated to simplify, in the embodiment of the present invention
The embodiment that the column length that part provide only stainless steel column is 150mm refers to for those skilled in the art.
The following detailed description of how with detection method provided by the invention come thiazine in parathiazine ketone-Mobucin compounding powder agent
The content of ketone and Mobucin determine simultaneously, and in the present embodiment, specific detection process comprises the following steps：
First, Preparatory work of experiment
1. the preparation of reagent, solution：
Methanol：Chromatographically pure；
Buprofezin standard specimen：Known quality fraction W >=98.0%；
Mobucin standard specimen：Known quality fraction W >=98.0%；
Water：It is new to steam redistilled water.
The preparation of standard specimen solution：Buprofezin standard specimen 0.05g is weighed respectively（It is accurate to 0.0002g）Mobucin 0.2g is (accurate
To 0.0002g), it is placed in 50ml volumetric flasks, adds methanol ultrasonic dissolution, scale is settled to after being cooled to room temperature.Accurately pipette this
Solution 5ml is placed in another 50ml volumetric flasks, is settled to scale with mobile phase, is shaken up, filtering.
The preparation of sample solution：Weigh 1.0g（It is accurate to 0.0002g）Sample, be placed in 50ml volumetric flasks, add methanol
Ultrasonic dissolution, scale is settled to after being cooled to room temperature.This solution 5ml is accurately pipetted in another 50ml volumetric flasks, uses mobile phase
Scale is settled to, is shaken up, is filtered.
2. the preparation of detecting instrument and equipment：
Liquid chromatograph：Has Variable wavelength UV detector；
Chromatographic data processor or chromatographic work station；
Chromatographic column：150mm×4.6mm（id）Stainless steel column, built-in Zirchrom C185 μm of fillers；
Filter：About 0.45 μm of filter sizes；
Microsyringe：50μL；
Quantitative sample injection pipe：5μL；
Ultrasonic cleaner.
2nd, liquid chromatogram operating condition
Mobile phase：ψ (methanol：Water)=70：30 (adjusting pH value=3 with phosphoric acid), through 0.45um membrane filtrations, and are de-gassed；
Mobile phase flow rate：0.8ml/min；
Column temperature：Room temperature (difference variation is less than 2 DEG C)；
Detector wavelength：225nm；
Sampling volume：5μL；
Retention time：Buprofezin 5.2min, Mobucin 6.7min.
It should be noted that aforesaid operations parameter is just for the present embodiment, it will be appreciated by those skilled in the art that, at this
In invention, it can be appropriately adjusted according to the characteristics of different instruments and chromatographic column, to reach optimum efficiency.
3rd, determine
Under the operating conditions described above, after instrumental baseline is stable, several pin standard specimen solutions is continuously injected into, treat adjacent two pins standard specimen
It is molten according to standard specimen solution, sample solution, sample when the relative change of Buprofezin/Mobucin peak area is respectively less than 1.0% in solution
Liquid, the order of standard specimen solution are measured.
4th, calculate
By the peak area of Buprofezin/Mobucin in two pin standard specimen solutions before and after the two pin sample solutions and sample that measure point
It is not averaged, the mass fraction W of Buprofezin/Mobucin in sample1, by formula（1）Calculate：
In formula：
A1--- in standard specimen solution, the average value of Buprofezin/Mobucin peak area；
A2--- in sample solution, the average value of Buprofezin/Mobucin peak area；
m1--- the quality of standard specimen, unit are gram（g）；
m2--- the quality of sample, unit are gram（g）；
W1--- the mass fraction of Buprofezin/Mobucin, numerical value are represented with % in standard specimen.
In the above-described embodiments, the liquid phase color of Buprofezin and Mobucin assay in Buprofezin-Mobucin compounding powder agent
Spectrogram is shown in Fig. 1, and 1 and 2 represent respectively in figure：1-Mobucin, 5.2min, 2-Buprofezin, 6.7min.
To verify whether detection method provided by the invention can meet the requirement of quantitative analysis and the essence of the detection method
Density and the degree of accuracy, its linear relationship, precision and the degree of accuracy are measured separately below.
The linear relationship measure of above-mentioned detection method：It is accurate to prepare 20.48ug/mL containing Buprofezin~307.2ug/mL, contain
Mobucin 89.2ug/mL~1337.4ug/mL various concentrations standard liquids, enter under operating condition as defined in above-mentioned detection method
Row measure, using concentration as abscissa, peak area is ordinate, and it is Y=65174.6x+85789 to obtain Buprofezin equation of linear regression
(n=5, r=0.9997), the equation of linear regression of Mobucin is Y=9737.2x+74247 (n=5, r=0.9999), and Buprofezin is surveyed
Fixed linear relationship chart is shown in Fig. 2, and Mobucin setting-out line sexual intercourse figure is shown in Fig. 3.
Analyzed more than, this detection method determines Buprofezin simultaneously, Mobucin is respectively provided with preferable linear relationship, energy
Meet the requirement of quantitative analysis.
The precision test and accuracy test result of above-mentioned detection method are shown in table 1 below, table 2 respectively.
The measure of the detection method precision of table 1
| Title | Measurement result % | Average value % | Standard deviation | Coefficient of variation % |
| Buprofezin | 5.22 5.26 5.27 5.05 5.21 5.07 | 5.18 | 0.096 | 1.85 |
| Mobucin | 20.20 20.09 20.35 20.25 20.39 20.19 | 20.24 | 0.11 | 0.55 |
The measure of the detection method degree of accuracy of table 2
It is above-mentioned while determine Buprofezin and Mobucin content in Buprofezin-Mobucin compounding powder agent from table 1, table 2
Method has preferably repeated, the higher degree of accuracy, the quality control being adapted in production.
In summary, detection method provided by the invention can realize other components in complex preparation within the faster time
Efficiently separated with Buprofezin, Mobucin, chromatogram peak symmetry is good, and sensitivity is higher, can realize Buprofezin-Mobucin compounding powder
Rapid and accurate determination while two kinds of Buprofezin, Mobucin active ingredient in agent, the assay method is simple to operate, analysis time
Short, testing result is accurate, is parathiazine ketone in production, the effective ways of Mobucin compounding powder agent progress quality control, is to instruct
The effective means that Buprofezin, Mobucin compounding powder agent normally produce.
Above-described embodiment is the preferable implementation of the present invention, and in addition, the present invention can be realized with other manner,
Any obviously replaced on the premise of not departing from the technical program design within protection scope of the present invention.
Finally it should be emphasised that in order to allow those of ordinary skill in the art more easily to understand the present invention relative to existing
There are the improvements of technology, some descriptions of the invention have been simplified, and for clarity, present specification is omitted
Some other elements, those of ordinary skill in the art should be aware that these elements omitted also may make up present disclosure.
Claims (1)
1. Buprofezin and the method for Mobucin content in Buprofezin-Mobucin compounding powder agent are determined simultaneously, it is characterised in that including
Following steps：
Prepare standard specimen solution and sample solution；The standard specimen solution is prepared using following methods：Buprofezin standard specimen is weighed respectively
0.05g, Mobucin standard specimen 0.2g, are placed in 50ml volumetric flasks, add methanol ultrasonic dissolution, scale is settled to after being cooled to room temperature,
This solution 5ml is accurately pipetted again to be placed in another 50ml volumetric flasks, scale is settled to mobile phase, shakes up, is filtered, and is weighed described
0.0002g is accurate to when Buprofezin standard specimen and Mobucin standard specimen；The sample solution is prepared using following methods：Weigh 1.0g's
Sample, it is placed in 50ml volumetric flasks, adds methanol ultrasonic dissolution, scale is settled to after being cooled to room temperature；Accurately pipette this solution 5ml
In another 50ml volumetric flasks, scale is settled to mobile phase, is shaken up, filtered, 0.0002g is accurate to when weighing the sample；
Then using filling Zirchrom C18The stainless steel column of 5 mu m bonded phase fillings and by phosphoric acid regulating ph value be 3 first
The mobile phase of alcohol+water carries out sample component separation, using high performance liquid chromatograph and UV-detector and using peak area external standard
Method carries out liquid chromatogram and quantitatively detected；
Methanol in the mobile phase：Water=70：30, the stainless steel column column length is 150mm, column internal diameter 4.6mm, described ultraviolet
Detector Detection wavelength is 225nm, and the mass fraction of Buprofezin and Mobucin is pressed in the Buprofezin Mobucin compounding powder agent
Following formula calculates：
<mrow>
<msub>
<mi>W</mi>
<mn>1</mn>
</msub>
<mo>=</mo>
<mfrac>
<mrow>
<msub>
<mi>A</mi>
<mn>2</mn>
</msub>
<mo>&CenterDot;</mo>
<msub>
<mi>m</mi>
<mn>1</mn>
</msub>
<mo>&CenterDot;</mo>
<mi>W</mi>
</mrow>
<mrow>
<msub>
<mi>A</mi>
<mn>1</mn>
</msub>
<mo>&CenterDot;</mo>
<msub>
<mi>m</mi>
<mn>2</mn>
</msub>
</mrow>
</mfrac>
<mo>;</mo>
</mrow>
In above formula, A1For in standard specimen solution, the average value of Buprofezin or Mobucin peak area；
A2For in sample solution, the average value of Buprofezin or Mobucin peak area；
m1For the quality of standard specimen, unit is gram (g)；
m2For the quality of sample, unit is gram (g)；
W1Represented for Buprofezin in standard specimen or the mass fraction of Mobucin, numerical value with percentage value.
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| CN104965035A (en) * | 2015-04-27 | 2015-10-07 | 公安部物证鉴定中心 | Method for screening toxic substances in sample by using solid phase support liquid-liquid extraction-GC MS |
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| CN104965035A (en) * | 2015-04-27 | 2015-10-07 | 公安部物证鉴定中心 | Method for screening toxic substances in sample by using solid phase support liquid-liquid extraction-GC MS |
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| 噻嗪酮•异丙威可湿性粉剂的高效液相色谱分析;张清泽 等;《农药科学与管理》;20061231;第27卷(第2期);第5-6页 * |
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