GB 28130-2011Pyridaben technical material (English PDF)

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. pore size of about 0.45µm;

Micro injector. 50µL;

Quantitative sample line. 5µL;

Ultrasonic cleaner.

4.3.1.4 HPLC operating conditions

Mobile phase. Psi (CH3CN.H2O) = 85.15;

Flow rate. 1.0mL/min;

Column temperature. room temperature (temperature change should not exceed 2 °C);

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

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 (°C). 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, rho (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 °C ~ 112 °C Vapor Pressure.