GB 28148-2011Pyridaben emulsifiable concentrates (English PDF)

3.1 Composition and appearance

This product should be compliant pyridaben the original drug formulated with an emulsifier dissolved in a suitable solvent, it should be stable homogeneous liquid, no Visible suspended solids and sediments.

3.2 Technical Specifications

Pyridaben EC shall comply with the requirements of Table 1.

Table 1 pyridaben EC Control Project Index

project

index

15% 20%

Pyridaben mass fraction /% 15.0 20.0 1.2-1.2 1.0 to 1.0 Moisture content /% <= 0.5 pH range of 4.5 to 8.5

Table 1 (continued)

project

index

15% 20%

Emulsion stability (diluted 200 times) Qualified Low temperature stability a qualified Thermal storage stability of a qualified when a normal production, heat storage stability test was measured at least once every three months.

Test Method 4

Safety Tips. Use of this standard shall have practical experience of laboratory personnel work. This standard does not point out all of the safety issues. Make with those who have the responsibility to take appropriate safety and health practices and to ensure compliance with the relevant national regulations.

4.1 General provisions

This standard reagents and water in the absence of other requirements specified, refers to three analytical reagent and GB/T 6682-2008 specified in water. Test results determined in accordance with GB/T 8170-2008 4.3.3 The "rounding value comparison method".

4.2 Sampling

According to GB/T 1605-2001 in "liquid formulations sampling" approach. Determining sample package using a random number table method; the final sample size not less than 250mL.

4.3 Identification Test

Gas Chromatography --- The identification test can be carried out simultaneously with the determination of the mass fraction of pyridaben. Under the same chromatographic operating conditions, the test A sample solution peak retention time compared with standard sample solution PYRIDABEN chromatographic retention time, the relative difference should be less than 1.5%.

Liquid chromatography --- The identification test can be carried out simultaneously with the determination of the mass fraction of pyridaben. Under the same chromatographic operating conditions, the test A sample solution peak retention time compared with standard sample solution PYRIDABEN chromatographic retention time, the relative difference should be less than 1.5%.

4.4 Determination of the mass fraction of pyridaben

4.4.1 High performance liquid chromatography (Arbitration Act)

4.4.1.1 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.

4.4.1.2 Reagents and solutions

Methanol;

Acetonitrile. chromatographic pure;

Water. The new secondary steam distilled water;

Pyridaben Sample. Known pyridaben mass fraction w>=99.0%.

4.4.1.3 Instruments

High performance liquid chromatography. a variable wavelength UV detector;

Chromatographic data processor or workstation;

Color 150mm × 3.9mm (id) stainless steel column, built-Nova-PakC18,5µm filler (or the equivalent effect. Column the column);

Filter. pore size of about 0.45µm;

Micro injector. 50µL;

Quantitative sample line. 5µL;

Ultrasonic cleaner.

4.4.1.4 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 EC HPLC is shown in Figure 1.

1 --- pyridaben.

Figure 1 pyridaben EC HPLC diagram

4.4.1.5 Measurement procedure

4.4.1.5.1 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.

4.4.1.5.2 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.

4.4.1.5.3 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.

4.4.1.6 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).

4.4.1.7 Allowable difference

Difference pyridaben mass fraction of two parallel determination results shall not be greater than 0.5%, the arithmetic mean value as a measurement result.

4.4.2 Capillary Gas Chromatography

4.4.2.1 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.

4.4.2.2 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.

4.4.2.3 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.

4.4.2.4 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 EC and the internal standard is shown in Figure 2.

1 --- internal standard;

2 --- pyridaben.

Figure 2 da gas chromatogram mites Ling EC and the internal standard

4.4.2.5 Measurement procedure

4.4.2.5.1 Preparation of standard solution

Weigh pyridaben standard 0.05g (accurate to 0.0002g), placed in a glass bottle stuffed with a pipette 5mL internal standard solution, Shake well.

4.4.2.5.2 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 4.4.2.5.1 with a pipette internal standard solution 5mL, shake.

4.4.2.5.3 Determination

Under the above chromatographic operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the peak two needles PYRIDABEN adjacent internal standard Changes in the relative area ratio is less than 1.5%, according to the solution, the sample solution, the sample solution and standard sequence analysis of the standard solution was measured.

4.4.2.6 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).

4.4.2.7 Allowable difference

The difference between two parallel determination results shall not be greater than 0.5%, the arithmetic mean value as a measurement result.

4.5 Determination of moisture content

According to GB/T 1600 the "Karl Fischer method".

Determination of 4.6 pH value According to GB/T 1601 carried out.

4.7 Emulsion stability test

Standard hard water sample was diluted 200-fold, according to GB/T 1603 test, no oil slick measuring cylinder (cream), and precipitation of heavy oil qualified.

4.8 Low temperature stability test

According to GB/T 19137 in "homogeneous emulsion and liquid preparations", in the bottom of the centrifuge tube educt volume does not exceed 0.3mL qualified.

4.9 Thermal storage stability test

According to GB/T 19136 in "liquid formulation" to. After the thermal storage, pyridaben mass fraction of not less than the average content measured before the heat storage 97%; emulsion stability should meet the standard requirements.

4.10 Product inspection and acceptance

Shall comply with GB/T 1604's.

5.1 Marking, labeling, packaging

Pyridaben EC marking, labeling and packaging should comply with the provisions of GB 4838. Pyridaben EC application of clean, dry glass or PET bottle packaging, bottle net content of 250mL (g), 100mL (g), external corrugated packaging, each box weighing no more than 10kg. also may According to user requirements or the order agreement, the use of other forms of packaging, subject to the provisions of GB 4838.

5.2 Storage

Pyridaben EC packages 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 Warranty Period

Under the provisions of storage and transportation conditions, the guarantee period pyridaben EC, two years from date of manufacture.

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.