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GB 28130-2011: [GB/T 28130-2011] Pyridaben technical material
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[GB/T 28130-2011] Pyridaben technical material
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Basic data | Standard ID | GB 28130-2011 (GB28130-2011) | | Description (Translated English) | [GB/T 28130-2011] Pyridaben technical material | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.10 | | Word Count Estimation | 11,130 | | Date of Issue | 2011-12-30 | | Date of Implementation | 2012-04-15 | | Quoted Standard | GB/T 601-2002; GB/T 1600; GB/T 1604; GB/T 1605-2001; GB 3796; GB/T 19138 | | Regulation (derived from) | Announcement of Newly Approved National Standards No. 23 of 2011 | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | | Summary | This Chinese standard specifies the Pyridaben drug requirements, test methods and marking, labeling, packaging, storage and acceptance period. This standard applies to Pyridaben impurities generated in the production and composition of Pyridaben original drug. | GB 28130-2011: [GB/T 28130-2011] Pyridaben technical material---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Pyridaben technical material
ICS 65.100.10
G25
National Standards of People's Republic of China
Pyridaben the original drug
Issued on. 2011-12-30
2012-04-15 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China released
Foreword
The standard Chapter 3, Chapter 5 is mandatory, the rest are recommended.
This standard was drafted in accordance with GB/T 1.1-2009 given rules.
Please note that some of the content of this document may involve patents. Release mechanism of the present document does not assume responsibility for the identification of these patents.
The standard proposed by China Petroleum and Chemical Industry Association.
This standard by the National Standardization Technical Committee on Pesticides (SAC/TC133) centralized.
This standard is drafted by. Shenyang Chemical Research Institute Co., Ltd.
It participated in the drafting of this standard. Jiangsu Suke Sheng Group Co., Ltd., Qingdao Otis biotechnology company.
The main drafters of this standard. Jiangmin Yi, Wu Wei, Wang Haixia, Decipher, Lixue Chen.
Pyridaben the original drug
1 Scope
This standard specifies the requirements, test methods and marking, labeling, packaging, storage and acceptance of pyridaben the original drug.
This standard applies to the impurities from the PYRIDABEN its production into the composition of pyridaben the original drug.
Note. Other name, structural formula and basic physicochemical parameters pyridaben see Appendix A.
2 Normative references
The following documents for the application of this document is essential. For dated references, only the dated version suitable for use herein
Member. For undated references, the latest edition (including any amendments) applies to this document.
Preparation of GB/T 601-2002 Chemical Reagent standard titration solution
GB/T 1600 Determination of Water Pesticides
GB/T 1604 Goods pesticide regulations for acceptance
GB/T 1605-2001 Sampling Method commercial pesticides
GB 3796 pesticide packaging General
GB/T 19138 Determination of pesticide insoluble in acetone (GB/T 19138-2003, CIPACMT27, MOD)
3 Requirements
3.1 Appearance
White granular or powdery solid, no visible foreign matter and filling the modifier.
3.2 Technical Specifications
Pyridaben the original drug should meet the requirements of Table 1.
Table 1 pyridaben the original drug control project indicators
Item Index
Pyridaben mass fraction /% ≥ 95.0
Moisture content /% ≤ 0.5
Acidity (H2SO4 meter) /% ≤
Or alkalinity (NaOH meter) /% ≤
0.3
0.2
Fraction a /% acetone insolubles ≤ 0.5 mass
When a normal production, acetone insoluble content was measured at least once every three months.
Test Method 4
4.1 Sampling
According to GB/T 1605-2001 "on the original drug product sampling" approach. Determined by sampling a random number table method packages, the final sample size
Not less than 100g.
4.2 Identification Test
You can choose one of the following methods. When not identify one way, then use another method should be determined.
Infrared spectroscopy --- sample and pyridaben standard infrared 4000cm-1 ~ 400cm-1 absorption spectrum should be no significant difference.
Pyridaben standard infrared spectrum is shown in Figure 1.
Figure 1 pyridaben standard infrared spectrum
HPLC --- The identification test can be carried out simultaneously with the determination of the mass fraction of pyridaben. In the same chromatographic operating conditions
, The sample solution to a chromatographic retention time and pyridaben standard solution PYRIDABEN chromatographic retention time, the relative difference should
1.5% or less.
4.3 Determination of the mass fraction of pyridaben
4.3.1 High performance liquid chromatography (Arbitration Act)
4.3.1.1 Method summary
Sample was dissolved in methanol, acetonitrile and water as the mobile phase, use as filler in Nova-PakC18 stainless steel column and UV detector
(240nm), the sample of PYRIDABEN high performance liquid chromatography and determination.
4.3.1.2 Reagents and solutions
Methanol;
Acetonitrile. chromatographic pure;
Water. The new secondary steam distilled water;
Pyridaben Sample. Known pyridaben mass fraction w≥99.0%.
4.3.1.3 Instruments
High performance liquid chromatography. a variable wavelength UV detector;
Chromatographic data processor or workstation;
Column. 150mm × 3.9mm (id) stainless steel column, built-Nova-PakC18,5μm filler (or equally effective column);
Filter. filter pore size of about 0.45μm;
Micro injector. 50μL;
Quantitative sample line. 5μL;
Ultrasonic cleaner.
4.3.1.4 HPLC operating conditions
Mobile phase. Ψ (CH3CN.H2O) = 85.15;
Flow rate. 1.0mL/min;
Column temperature. room temperature (temperature change should not exceed 2 ℃);
Detection wavelength. 240nm;
Injection volume. 5μL;
Retention time. pyridaben about 5.6min.
It said operating parameters are typical, according to the characteristics of different instruments, given operating parameters adjusted as appropriate, in order to obtain the best results.
Typical pyridaben the original drug HPLC is shown in Figure 2.
1 --- pyridaben.
Figure 2 HPLC pyridaben the original drug
4.3.1.5 Measurement procedure
4.3.1.5.1 Preparation of standard solution
Weigh 0.1g PYRIDABEN standard (accurate to 0.0002g), a 50mL volumetric flask, dilute to the mark with methanol, ultrasonic oscillation
5min make sample dissolution, cooled to room temperature and shake well. Using a pipette to take the above solution 5mL to 50mL volumetric flask, diluted with methanol
To the mark.
4.3.1.5.2 Preparation of sample solution
Weigh containing pyridaben 0.1g sample (accurate to 0.0002g), a 50mL volumetric flask, dilute to the mark with methanol, ultrasonic
Oscillation 5min make sample dissolution, cooled to room temperature and shake well. Using a pipette to take the above solution 5mL to 50mL volumetric flask with methanol
Dilute to the mark.
4.3.1.5.3 Determination
Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles PYRIDABEN Lingfeng area relative change
After less than 1.2%, according to the solution, the sample solution, the sample solution and standard sequence of the standard solution was measured.
4.3.1.6 Calculation
The two needle sample solution and measured before and after the two doses of the standard sample solution PYRIDABEN Lingfeng area were averaged. Sample PYRIDABEN
The mass fraction according to equation (1).
w1 = A2
· M1 · w
A1 · m2
(1)
Where.
w1 --- sample pyridaben mass fraction, expressed as a percentage;
A2 --- sample solution, pyridaben mean Lingfeng area;
m1 --- pyridaben standard mass in grams (g);
w --- pyridaben standard mass fraction, expressed as a percentage;
A1 --- standard solution, pyridaben mean Lingfeng area;
m2 --- sample mass, in grams (g).
4.3.1.7 allowable difference
Difference pyridaben mass fraction of two parallel determination results shall not be greater than 1.2%, the arithmetic mean value as a measurement result.
4.3.2 Capillary Gas Chromatography
4.3.2.1 Method summary
Sample was dissolved in chloroform, dicyclohexyl phthalate esters as internal standard, using a DB-1701 capillary column coated walls, and hydrogen
Flame ionization detector, sample the PYRIDABEN capillary gas chromatography and determination.
4.3.2.2 Reagents and solutions
Chloroform;
Pyridaben standard. a known mass fraction w≥99.0%;
Dicyclohexyl phthalate ester. not interfere with the analysis of impurities;
Internal standard solution. Weigh 5.0g dicyclohexyl phthalate esters into 500mL volumetric flask, dissolved with chloroform, constant volume,
Shake well.
4.3.2.3 Instruments
Gas chromatograph. with flame ionization detector;
Column. 30m × 0.32mm (id) quartz capillary column, wall coated with DB-1701, a film thickness of 0.25μm;
Chromatographic data processor or chromatography workstation.
4.3.2.4 GC operating conditions
Temperature (℃). Room 240 column, the gasification chamber 270, detection chamber 280;
Gas flow rate (mL/min). carrier gas (N2) 1.8, hydrogen gas 30, air 300, the compensation gas 25;
Split ratio. 40.1;
Injection volume. 2.0μL;
Retention time. pyridaben about 8.2min, internal standard about 5.0min.
GC operating conditions described above, the Department of typical operating parameters. According to the characteristics of different instruments, given operating parameters adjusted as appropriate,
In order to obtain the best results. A typical gas chromatogram pyridaben the original drug and the internal standard are shown in Figure 3.
1 --- internal standard;
2 --- pyridaben.
Figure 3 pyridaben the original drug and the internal standard gas chromatograph
4.3.2.5 Measurement procedure
4.3.2.5.1 preparation of standard solution
Weigh pyridaben standard 0.05g (accurate to 0.0002g), placed in a glass bottle stopper, with a pipette accurately added internal standard solution 5mL
Liquid, shake.
4.3.2.5.2 preparation of the sample solution
Weigh containing pyridaben 0.05g sample (accurate to 0.0002g), placed in a glass bottle stopper, with the use and 4.3.2.5.1
With a pipette accurately added internal standard solution 5mL, shake.
4.3.2.5.3 Determination
Under the above chromatographic operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles pyridaben and the internal standard
After the change of the relative peak area ratio of less than 1.5%, according to the solution, the sample solution, the sample solution and standard sequence analysis of the standard solution
Determination.
4.3.2.6 Calculation
The two needle sample solution and measured before and after the two doses of the standard sample solution PYRIDABEN and the internal standard peak area ratios are averaged.
Sample PYRIDABEN content according to formula (1 ') Calculated.
w'1 = r2 × m1 × wr1 × m2
(1')
Where.
w'1 --- sample PYRIDABEN mass fraction, expressed as a percentage;
r2 --- the average of the sample solution PYRIDABEN and the internal standard peak area ratio;
m1 --- standard mass in grams (g);
w --- standard samples pyridaben mass fraction, expressed as a percentage;
Mites and the average internal standard peak area ratio r1 --- standard solution clatter;
m2 --- sample mass, in grams (g).
4.3.2.7 allowable difference
The difference between two parallel determination results shall not be greater than 1.2%, the arithmetic mean value as a measurement result.
4.4 Determination of moisture content
According to GB/T 1600 carried out. Allow the use of equivalent accuracy trace moisture analyzer.
4.5 Determination of acidity (alkalinity) mass fraction
4.5.1 Reagents and solutions
Sodium hydroxide standard titration solution c (NaOH) = 0.02mol/L, according to GB/T 601-2002 4.1 preparation and calibration;
Hydrochloric acid standard volumetric solution c (HCl) = 0.02mol/L, according to GB/T 601-2002 4.1 preparation and calibration;
Indicator solution. bromocresol green ethanol solution, ρ (bromocresol green) = 1g/L;
Acetone solution. Take 10mL of water and 90mL acetone, add indicator solution 1mL, shake. Titration with sodium hydroxide standard titration solution from yellow
Color to blue, set aside.
4.5.2 Determination
Weigh the sample 1g (accurate to 0.002g), placed in a 150mL conical flask, acetone solution 25mL, shake to dissolve the sample.
If the solution is yellow by a) determining the acidity of the solution; if the solution is blue press b) determining the alkalinity of the solution.
a) Acidity. with 0.02mol/L sodium hydroxide standard titration solution, titration, titrate the solution to the blue end.
b) alkalinity. with 0.02mol/L hydrochloric acid standard titration solution titration, titrate the solution to yellow as the end point.
4.5.3 Calculation
a) a sample of acidity according to formula (2).
w2 = cV1 × Mm × 1000 × 100
(2)
Where.
w2 --- sample acidity, expressed as a percentage;
C --- the actual concentration of sodium hydroxide standard titration solution, expressed in moles per liter (mol/L);
Volume V1 --- titration of the sample solution consumed sodium hydroxide standard titration solution, in milliliters (mL);
--- The M values of the molar mass of sulfuric acid, in units of grams per mole (g/mol), M 12H2SO
÷ 4
êê
úú = 49;
M --- the quality of the sample, in grams (g).
b) Sample alkalinity according to formula (2 ') Calculated.
w'2 = cV1 × Mm × 1000 × 100
(2')
Where.
w'2 --- sample alkalinity, expressed as a percentage;
C --- the actual concentration of hydrochloric acid standard titration solution, expressed in moles per liter (mol/L);
Volume V1 --- titration of the sample solution consumption hydrochloric acid standard titration solution, in milliliters (mL);
--- The M NaOH numerical molar mass in grams per mole (g/mol), [M (NaOH) = 40];
M --- the quality of the sample, in grams (g).
4.6 Determination of acetone insoluble mass fraction
According to GB/T 19138 performed.
4.7 product testing and acceptance
Shall comply with GB/T 1604 regulations limit the use of numerical processing rounding value comparison method.
5 marking, labeling, packaging, storage, security, acceptance of
5.1 marking, labeling, packaging
Flag pyridaben the original drug, labeling, packaging shall comply with the provisions of GB 3796; pyridaben the original drug use bags lined with clean plastic bag
Or cardboard lined with clean plastic bag, net weight per barrel is generally 25kg; it can be used according to user requirements or order agreement
Other forms of packaging, subject to the provisions of GB 3796.
5.2 Storage
Pyridaben the original drug package should be stored in ventilated, dry warehouse; storage and transportation to prevent moisture and sunlight, no food, seed, feed
Mix, avoid contact with skin, eyes, mouth and nose to prevent inhalation.
5.3 Security
This product is moderately toxic mites, pesticides, are swallowed and inhaled toxic, can penetrate through the skin. Wear protective goggles and rubber the FDA
Leather gloves to wear the necessary protective clothing. After application, immediately wash with soap and water. Such as skin, eyes accidentally stained the product immediately with large
The amount of rinse. Coverage should be immediately sent to hospital symptomatic treatment.
5.4 Acceptance of
Pyridaben the original drug acceptance period is one month. From the date of delivery, the quality of the finished product acceptance within one month, the indicators should be consistent
standard requirement.
Appendix A
(Informative)
Pyridaben other name, structural formula and basic physicochemical parameters
This product is an active ingredient pyridaben other name, structural formula and basic physicochemical parameters are as follows.
ISO common name. Pyridaben
CAS Registry Number. 96489-71-3
CIPAC Numeric Code. 583
Chemical name. 2-tert-butyl-5- (4-tert-butyl-benzyl) -4-chloro -3 (2H) - pyridazinone
Structure.
Empirical formula. C19H25ClN2OS
Molecular Weight. 364.9
Biological activity. acaricidal, insecticidal
Melting point. about 111 ℃ ~ 112 ℃
Vapor Pressure. < 0.25mPa (20 ℃)
Solubility (20 ℃, g/L). water, 1.2 × 10-5, 460 acetone, benzene, 110, 320 cyclohexane, 57 ethanol, n-octane 63, hexanes 10, two
Toluene 390
Stability. aqueous solution pH4 ~ pH9 and most organic solvents stable, 50 ℃ storage stable for three months under normal storage conditions
At least two years is stable, unstable to light.
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ISBN. 155 066 · 1-44787
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