CN104020223B - A kind of analytical approach of S-methoprene massfraction - Google Patents
A kind of analytical approach of S-methoprene massfraction Download PDFInfo
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- CN104020223B CN104020223B CN201410148341.3A CN201410148341A CN104020223B CN 104020223 B CN104020223 B CN 104020223B CN 201410148341 A CN201410148341 A CN 201410148341A CN 104020223 B CN104020223 B CN 104020223B
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- NFGXHKASABOEEW-UHFFFAOYSA-N 1-methylethyl 11-methoxy-3,7,11-trimethyl-2,4-dodecadienoate Chemical compound COC(C)(C)CCCC(C)CC=CC(C)=CC(=O)OC(C)C NFGXHKASABOEEW-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 238000013459 approach Methods 0.000 title claims abstract description 11
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229950003442 methoprene Drugs 0.000 claims abstract description 36
- 150000002148 esters Chemical class 0.000 claims abstract description 25
- 229930002897 methoprene Natural products 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000004811 liquid chromatography Methods 0.000 claims abstract description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000004817 gas chromatography Methods 0.000 claims abstract description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 6
- -1 polysiloxane Polymers 0.000 claims abstract description 6
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 6
- 238000004090 dissolution Methods 0.000 claims abstract description 3
- 238000010828 elution Methods 0.000 claims abstract description 3
- 238000010812 external standard method Methods 0.000 claims abstract description 3
- 239000000523 sample Substances 0.000 claims description 47
- 239000000243 solution Substances 0.000 claims description 25
- 239000012488 sample solution Substances 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 15
- 230000005477 standard model Effects 0.000 claims description 15
- 238000010790 dilution Methods 0.000 claims description 14
- 239000012895 dilution Substances 0.000 claims description 14
- 238000012360 testing method Methods 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N isopropyl alcohol Natural products CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 230000014759 maintenance of location Effects 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 6
- NFGXHKASABOEEW-UQHDCKCOSA-N (R)-methoprene Chemical compound COC(C)(C)CCC[C@@H](C)C\C=C\C(\C)=C\C(=O)OC(C)C NFGXHKASABOEEW-UQHDCKCOSA-N 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 239000006199 nebulizer Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 239000006200 vaporizer Substances 0.000 claims description 3
- DYLIWHYUXAJDOJ-OWOJBTEDSA-N (e)-4-(6-aminopurin-9-yl)but-2-en-1-ol Chemical compound NC1=NC=NC2=C1N=CN2C\C=C\CO DYLIWHYUXAJDOJ-OWOJBTEDSA-N 0.000 claims description 2
- NFGXHKASABOEEW-LDRANXPESA-N methoprene Chemical compound COC(C)(C)CCCC(C)C\C=C\C(\C)=C\C(=O)OC(C)C NFGXHKASABOEEW-LDRANXPESA-N 0.000 claims 10
- 238000002347 injection Methods 0.000 claims 1
- 239000007924 injection Substances 0.000 claims 1
- 239000012086 standard solution Substances 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 3
- 241000238631 Hexapoda Species 0.000 description 2
- 238000012790 confirmation Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000011003 system suitability test Methods 0.000 description 2
- 241000255925 Diptera Species 0.000 description 1
- 241000257232 Haematobia irritans Species 0.000 description 1
- 241000382353 Pupa Species 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 210000003484 anatomy Anatomy 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 210000002251 corpora allata Anatomy 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003630 growth substance Substances 0.000 description 1
- 239000003668 hormone analog Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 229930014550 juvenile hormone Natural products 0.000 description 1
- 239000002949 juvenile hormone Substances 0.000 description 1
- 150000003633 juvenile hormone derivatives Chemical class 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000006340 racemization Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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Abstract
The invention discloses a kind of analytical approach of S-methoprene massfraction, comprise the mensuration of the total ester of methoprene (trans) content and the mensuration of S-methoprene S/R ratio and S-methoprene massfraction; Namely sample toluene dissolves, use capillary chromatographic column and fid detector that 5% phenyl-95% methyl polysiloxane is immobile liquid, gas chromatography separated island form is carried out to the methoprene in sample, uses external standard method to calculate the total ester of methoprene (trans) content; Sample n-hexane dissolution, uses Chiral liquid chromatography post and positive elution system, carries out chiral chromatogram separated island form, determine S-methoprene S/R ratio according to peak area percent to the methoprene in sample.In the total ester of methoprene (trans) content and S-methoprene, the product of S body ratio is the massfraction of S-methoprene.
Description
Technical field
The present invention relates to analysis field, particularly relate to a kind of analytical approach of S-methoprene massfraction.
Background technology
S-methoprene ［ CAS:65733-16-6 ］, belong to corpus allatum hormone analog, structural formula is as follows:
S-methoprene belongs to insect growth regulator, IGR, and it does not directly kill larva or adult with toxicity, but acts on larva with juvenile hormone, and larva will rest on the worm pupa stage, successfully can not sprout wings and become adult.In view of the above-mentioned mechanism of action, the growth course of insect is suppressed, to reach deinsectization object.This product is applicable to mosquito, horn fly, flea, louse, the control of grain storage pest, and effectively employs abroad and reach 30 years.
In S-methoprene structure, 7 have 1 chiral center, and 2 double bonds exist cis-trans-isomer, and 4 double bonds exist with transconfiguration, and the trans isomerization being transformed into cis very easily occurs 2 cis-trans isomerism types.
4 isomers tables specific as follows of S-methoprene:
In 4 isomerss, only having S-methoprene (trans) to be effective ingredient, is also the S-methoprene of indication of the present invention.
Summary of the invention
An analytical approach for S-methoprene massfraction, is characterized in that: comprise following mensuration:
1) mensuration of the total ester of methoprene (trans) content
Sample toluene dissolves, use capillary chromatographic column and fid detector that 5% phenyl-95% methyl polysiloxane is immobile liquid, gas chromatography separated island form is carried out to the methoprene in sample, uses external standard method to calculate the total ester of methoprene (trans) content.
2) mensuration of S-methoprene S/R ratio and S-methoprene massfraction
Sample n-hexane dissolution, uses Chiral liquid chromatography post and positive elution system, carries out chiral chromatogram separated island form, determine S-methoprene S/R ratio according to peak area percent to the methoprene in sample.In the total ester of methoprene (trans) content and S-methoprene, the product of S body ratio is the massfraction of S-methoprene.
Described 1), its instrument condition:
Gas chromatograph: there is fid detector:
Chromatographic work station:
Chromatographic column: 30m × 0.25mm (i.d) bore capillary tube post, is coated with 5% phenyl-95% methyl polysiloxane immobile liquid coating of 1.0um thickness:
Ultrasonic oscillator:
Described gas chromatography operating conditions is as follows:
Column temperature: 80 DEG C/0 minute-6.5 DEG C/min-300 DEG C/6 minutes;
Injector temperature: (vaporizer temperature): 280 DEG C;
Detected temperatures: (sensing chamber's temperature): 300 DEG C;
Carrier gas: High Purity Nitrogen;
Nebulizer gas pressure: 25psi;
Split ratio: 10.2/1;
Air mass flow: 300ml/min;
Hydrogen flowing quantity: 30ml/min;
Sampling volume: 0.1ul;
Relative retention time: methoprene trans-isomer: 1.00;
Methoprene cis-isomer: 0.96.
Described 1) determination step is as follows:
The preparation of A, standard specimen solution:
Take 0.5gS-methoprene standard model, by dilution with toluene and constant volume to 10ml, ultrasonic vibration 1min is for subsequent use.
The preparation of B, sample solution:
Take 0.5gS-methoprene specimen sample, by dilution with toluene and constant volume to 10ml, ultrasonic vibration 1min is for subsequent use.
C, mensuration:
Under the operating conditions described above, after instrumental baseline is stable, inject number pin mark sample solution continuously, until phase
Connect two pins, methoprene (trans) peak area relatively changes and is less than 5%, first injects toluene solvant as blank, then tests according to standard specimen solution, sample solution, sample solution, standard specimen solution order.
Described 1) the total ester of methoprene (trans) cubage is as follows:
The total ester of a, methoprene (trans) content C
(total ester)(%), calculate by formula (1):
In formula:
A
1: the total ester of methoprene (trans) peak area in standard model;
A
2: the total ester of methoprene (trans) peak area in test sample;
M
1: the weigh of standard model;
M
2: the weigh of test sample;
T: the total ester of methoprene (trans) content of standard model, %, known quality mark;
Described 2), in, its instrument condition is:
High performance liquid chromatograph: there is variable wavelength UV detecting device;
Chromatographic work station;
Chromatographic column: 250mm × 4.6mm (i.d) stainless steel column, in-built Daicel chiralpakAD-Hsilica, 5um filling material;
Ultrasonator.
The operating conditions of described liquid chromatography:
Mobile phase: count by volume: normal hexane/isopropyl alcohol=100/0.5;
Flow: 0.5ml/min;
Determined wavelength: 254nm;
Column temperature: 25 DEG C;
Sampling volume: 10.0ul;
Relative retention time: S-methoprene: 1.00;
R-methoprene: 1.06;
Described 2) determination step:
The preparation of A, standard specimen solution:
Take 20mgS-methoprene standard model, with mobile phase dilution constant volume to 10ml, then draw this solution 0.1ml, still dilute constant volume to 10ml, ultrasonic vibration 1min with mobile phase, for subsequent use;
The preparation of B, sample solution:
Take 20mgS-methoprene testing sample, with mobile phase dilution constant volume to 10ml, then draw this solution 0.1ml, still dilute constant volume to 10ml, ultrasonic vibration 1min with mobile phase, for subsequent use;
C, mensuration:
Under the operating conditions described above, after instrumental baseline is stable, inject number pin mark sample solution continuously, until two pins that are connected, S-methoprene peak area relatively changes and is less than 5%, tests according to standard specimen solution, sample solution, sample solution, standard specimen solution order.
Described 2) being calculated as follows of S-methoprene massfraction and methoprene S/R ratio E in:
(1) S-methoprene massfraction C
(S-methoprene)(%), calculate by formula (3):
In formula:
AS:S-methoprene peak area;
AR:R-methoprene peak area;
C (total ester): the total ester of methoprene (trans) content;
(2) methoprene S/R ratio E, calculates by formula (4):
In formula:
QS:S-methoprene peak area ratio, QS=AS/ (AS+AR) × 100%;
QR:R-methoprene peak area ratio, QR=AR/ (AS+AR) × 100%.
Beneficial effect of the present invention is:
The invention provides a kind of analytical approach of S-methoprene massfraction, the method is by the effective constituent of S-methoprene, and impurity has carried out thorough anatomy, has the meaning that the world is pioneering.Meanwhile, specify that the composition of S-methoprene, to Instructing manufacture, system product standard provides strong foundation.
Accompanying drawing explanation
Fig. 1 is methoprene gas chromatogram;
Fig. 2 is racemization methoprene chiral separation liquid chromatography figure;
Fig. 3 is S-methoprene chiral separation liquid chromatography figure;
Fig. 4 is S-methoprene gas phase analysis linear graph.
Specific embodiment
Below by specific embodiment, the present invention is described in detail.
embodiment 1
One, instrument condition
1, instrument configuration:
Gas chromatograph: there is fid detector;
Chromatographic work station;
Chromatographic column: 30m × 0.25mm (i.d) bore capillary tube post, is coated with 5% phenyl-95% methyl polysiloxane immobile liquid coating of 1.0um thickness;
Ultrasonic oscillator.
2, chromatographic condition:
Column temperature: 80 DEG C/0 minute-6.5 DEG C/min-300 DEG C/6 minutes;
Injector temperature: (vaporizer temperature): 280 DEG C;
Detected temperatures: (sensing chamber's temperature): 300 DEG C;
Carrier gas: High Purity Nitrogen;
Nebulizer gas pressure: 25psi;
Split ratio: 10.2/1;
Air mass flow: 300ml/min;
Hydrogen flowing quantity: 30ml/min;
Sampling volume: 0.1ul;
One, system suitability test
1, sample preparation:
Accurately take the S-methoprene standard model of 500mg (being accurate to 0.1mg), with dilution with toluene constant volume to 10mL.
2, sample introduction:
By the standard model solution for preparing continuous sample introduction three times under the chromatographic condition of regulation, record S-methoprene each time goes out peak retention time and peak area, carries out system suitability test.
Two, linear relationship
1, sample preparation:
Take the S-methoprene standard model of following weight, with dilution with toluene constant volume to 10mL, and identified as samples is designated as X1 ~ X6;
350mg，400mg，450mg，500mg，550mg，600mg；
2, sample introduction: X1 ~ X6 six samples sample introduction respectively, each sample feeding twice;
3, sample introduction record
4, interpretation of result
Linear analysis result shows, S-methoprene sample concentration has the good range of linearity between 35.12 ~ 59.93g/L.Equation of linear regression is Y=581.68X-9582.5, coefficient R=0.9997.
Three, the confirmation of accuracy
1, sample preparation
Within the scope of 350 ~ 600mg, take the S-methoprene standard model of constant weight at random, with dilution with toluene constant volume to 10mL, and identified as samples is designated as Z1 ~ Z6;
Choose X4 solution as standard solution;
2, sample introduction: Z1 ~ Z6 six samples sample introduction respectively, each sample feeding twice, according to the order sample introduction of a pin standard solution, two sample needle solution, a pin standard solution;
3, sample introduction record
4, interpretation of result
The gained recovery, between 99.0% ~ 101.0%, meets accuracy and confirms requirement;
Four, the confirmation of system precision
1, sample preparation
Take six test samples, example weight is 500mg, with dilution with toluene constant volume to 10mL, and identified as samples is designated as J1 ~ J6; Choose X4 solution as standard solution;
2, sample introduction: J1 ~ J6 six samples sample introduction respectively, each sample feeding twice, according to the order sample introduction of a pin standard solution, two sample needle solution, a pin standard solution, carries out cubage according to formula;
3, sample introduction record
4. interpretation of result
Relative standard deviation is 0.13%, shows that the precision of system meets the requirements;
The ratio measuring of S body in S-methoprene:
One, instrument condition
High performance liquid chromatograph: there is variable wavelength UV detecting device;
Chromatographic work station;
Chromatographic column: 250mm × 4.6mm (i.d) stainless steel column, in-built Daicel chiralpakAD-Hsilica, 5um filling material;
Ultrasonator;
Two, the operating conditions of liquid chromatography:
Mobile phase: normal hexane/isopropyl alcohol=100/0.5 (volume ratio);
Flow: 0.5ml/min;
Determined wavelength: 254nm;
Column temperature: 25 DEG C;
Sampling volume: 10.0ul;
Relative retention time: S-methoprene: 1.00;
R-methoprene: 1.06;
Three, determination step:
1, sample preparation
The preparation of A, standard specimen solution
Take 20mgS-methoprene standard model, with mobile phase dilution constant volume to 10ml, then draw this solution 0.1ml, still dilute constant volume to 10ml, ultrasonic vibration 1min with mobile phase, for subsequent use;
The preparation of B, test solution
Take the S-methoprene test sample corresponding to 20mgJ1-J6 respectively, with mobile phase dilution constant volume to 10ml, then draw this solution 0.1ml, still dilute constant volume to 10ml, ultrasonic vibration 1min with mobile phase, and identified as samples is designated as S1 ~ S6;
2, sample introduction:
S1 ~ S6 six samples sample introduction respectively, each sample feeding twice, according to the order sample introduction of a pin standard solution, two sample needle solution, a pin standard solution, direct reference area degree;
3. sample introduction record
S-methoprene massfraction (%)
Claims (5)
1. an analytical approach for S-methoprene massfraction, is characterized in that: comprise following mensuration:
1) mensuration of trans methoprene total ester content
Sample toluene dissolves, and uses capillary chromatographic column and fid detector that 5% phenyl-95% methyl polysiloxane is immobile liquid, carries out gas chromatography separated island form to the methoprene in sample, uses external standard method to calculate trans methoprene total ester content;
2) mensuration of S-methoprene S/R ratio and S-methoprene massfraction
Sample n-hexane dissolution, uses Chiral liquid chromatography post and positive elution system, carries out chiral chromatogram separated island form, determine S-methoprene S/R ratio according to peak area percent to the methoprene in sample;
In trans methoprene total ester content and S-methoprene, the product of S body ratio is the massfraction of S-methoprene;
Described 1), its instrument condition:
Gas chromatograph: there is fid detector;
Chromatographic work station:
Chromatographic column: 30m × 0.25mm (i.d) bore capillary tube post, is coated with 5% phenyl-95% methyl polysiloxane immobile liquid coating of 1.0 μm of thickness;
Ultrasonic oscillator;
Described gas chromatography operating conditions is as follows:
Column temperature: 80 DEG C/0 minute-6.5 DEG C/min-300 DEG C/6 minutes;
Injector temperature: vaporizer temperature: 280 DEG C;
Detected temperatures: sensing chamber's temperature: 300 DEG C;
Carrier gas: High Purity Nitrogen;
Nebulizer gas pressure: 25psi;
Split ratio: 10.2/1;
Air mass flow: 300ml/min;
Hydrogen flowing quantity: 30ml/min;
Sampling volume: 0.1 μ l;
Relative retention time: methoprene trans-isomer: 1.00;
Methoprene cis-isomer: 0.96;
Described 2), in, its instrument condition is:
High performance liquid chromatograph: there is variable wavelength UV detecting device;
Chromatographic work station;
Chromatographic column: 250mm × 4.6mm (i.d) stainless steel column, in-built Daicel chiralpakAD-Hsilica, 5 μm of filling materials;
Ultrasonator;
The operating conditions of described liquid chromatography:
Mobile phase: count by volume: normal hexane/isopropyl alcohol=100/0.5;
Flow: 0.5ml/min;
Determined wavelength: 254nm;
Column temperature: 25 DEG C;
Sampling volume: 10.0 μ l;
Relative retention time: S-methoprene: 1.00;
R-methoprene: 1.06.
2. the analytical approach of a kind of S-methoprene massfraction according to claim 1, is characterized in that, described 1) determination step as follows:
The preparation of A, standard specimen solution:
Take 0.5gS-methoprene standard model, by dilution with toluene and constant volume to 10ml, ultrasonic vibration 1min is for subsequent use;
The preparation of B, sample solution:
Take 0.5gS-methoprene specimen sample, by dilution with toluene and constant volume to 10ml, ultrasonic vibration 1min is for subsequent use;
C, mensuration:
Under gas chromatography operating conditions, after instrumental baseline is stable, continuous injection number pin mark sample solution, two pins until be connected, trans methoprene peak area relatively changes and is less than 5%, first inject toluene solvant as blank, then test according to standard specimen solution, sample solution, sample solution, standard specimen solution order.
3. the analytical approach of a kind of S-methoprene massfraction according to claim 1, is characterized in that, described 1) trans methoprene total ester content is calculated as follows:
A, trans methoprene total ester content C
(total ester)(%), calculate by formula (1):
In formula:
A
1: the total ester peak area of trans methoprene in standard model;
A
2: the total ester peak area of trans methoprene in test sample;
M
1: the weigh of standard model;
M
2: the weigh of test sample;
T: the trans methoprene total ester content of standard model, %, known quality mark.
4. the analytical approach of a kind of S-methoprene massfraction according to claim 1, is characterized in that: determination step described 2):
The preparation of A, standard specimen solution:
Take 20mgS-methoprene standard model, with mobile phase dilution constant volume to 10ml, then draw this solution 0.1ml, still dilute constant volume to 10ml, ultrasonic vibration 1min with mobile phase, for subsequent use;
The preparation of B, sample solution:
Take 20mgS-methoprene testing sample, with mobile phase dilution constant volume to 10ml, then draw this solution 0.1ml, still dilute constant volume to 10ml, ultrasonic vibration 1min with mobile phase, for subsequent use;
C, mensuration:
Under the operating conditions of liquid chromatography, after instrumental baseline is stable, inject number pin mark sample solution continuously, until two pins that are connected, S-methoprene peak area relatively changes and is less than 5%, tests according to standard specimen solution, sample solution, sample solution, standard specimen solution order.
5. the analytical approach of a kind of S-methoprene massfraction according to claim 1, is characterized in that: being calculated as follows of S-methoprene massfraction and methoprene S/R ratio E described 2):
(1) S-methoprene massfraction C
(S-methoprene)(%), calculate by formula (3):
In formula:
A
s: S-methoprene peak area;
A
r: R-methoprene peak area;
C
(total ester): trans methoprene total ester content;
(2) methoprene S/R ratio E, calculates by formula (4):
In formula:
Q
s: S-methoprene peak area ratio, Q
s=A
s/ (A
s+ A
r) × 100%;
Q
r: R-methoprene peak area ratio, Q
r=A
r/ (A
s+ A
r) × 100%.
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| CN106706824B (en) * | 2015-11-16 | 2018-04-13 | 中国科学院大连化学物理研究所 | The detection method of juvenile hormone JH II in a kind of insect bodies of application of gas chromatorgraphy/mass |
| CN109959730A (en) * | 2017-12-26 | 2019-07-02 | 广东东阳光药业有限公司 | A method of with the related substance of HPLC method measurement methoprene |
| CN108279273A (en) * | 2017-12-28 | 2018-07-13 | 常州胜杰化工有限公司 | A kind of HPLC analytical method of S- hydroprenes |
| CN112219862A (en) * | 2020-10-13 | 2021-01-15 | 博益德（北京）生物科技有限公司 | Fly and larva killing agent for farm |
| WO2023123194A1 (en) * | 2021-12-30 | 2023-07-06 | 浙江海正药业股份有限公司 | Analysis method for detecting chiral isomer impurities in methoprene |
| CN114460204B (en) * | 2022-02-15 | 2023-04-07 | 梅里埃检测技术(青岛)有限公司 | Method for simultaneously detecting cyenopyrafen and methoprene pesticide residues in plant-derived food |
| CN114624365B (en) * | 2022-04-18 | 2023-08-08 | 中国测试技术研究院 | Method for simultaneously determining residues of three methoprene juvenile hormone analogues in tea |
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| Isocratic reversed-phase liquid chromatographic method for the simultaneous determination of (S)-methoprene, MGK264, piperonyl butoxide, sumithrin and permethrin in pesticide formulation;I-Hsiung Wang等;《Journal of Chromatography A》;20031231;第983卷;第145-152页 * |
| 烯虫酯的立体选择性全合成;周容等;《有机化学》;20081231;第28卷(第3期);第436-439页 * |
| 高效液相色谱法测定蔬菜和粮食中的烯虫酯;徐爱平等;《化学分析计量》;20091231;第18卷(第1期);第33-35页 * |
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