GB 22624-2008Prochloraz emulsifiable concentrates (English PDF)

3.1 Composition and appearance

This product should be compliant prochloraz original drug is made into a stable homogeneous liquid, free from visible suspended matter and sediment.

3.2 Technical Specifications

Prochloraz EC shall comply with the requirements of Table 1.

Table 1 Prochloraz EC Control Project Index

project

index

25% 45% 450g/L

Prochloraz mass fraction a /% or concentration/(g/L) 25.0 + 45.0 + 2.2-2.2 1.5-1.5 2.1-2.1 42.0 + - - + 22-22 450 2,4,6-trichlorophenol mass fraction b /% <= 0.2 0.3 Moisture content /% <= 0.5 a pH range of 5.5 to 8.5 Emulsion stability (diluted 200 times) Qualified Low temperature stability Qualified b Thermal storage stability b qualified when a dispute occurs when mass to the mass fraction of arbitration.

B when normal production of 2,4,6-trichlorophenol, thermal storage stability test, measuring low temperature stability test at least once every three months.

Test Method 4

4.1 Sampling

According to GB/T 1605-2001 in "liquid formulations sampling" approach. Determined by sampling a random number table method packages, the final sample size not less than 200mL.

4.2 Identification Test

HPLC --- The identification test can be carried out simultaneously with the determination of the mass fraction of prochloraz. In the same chromatographic operating conditions , The sample solution to a chromatographic retention time of the standard solution PROCHLORAZ chromatographic retention time, the relative difference should be 1.5% Fewer.

4.3 Determination of the mass fraction of prochloraz

4.3.1 Method summary

Sample was dissolved in methanol, acetonitrile + methanol + water as the mobile phase, to use as filler AgilentTC-C18 stainless steel column and ultraviolet Detector (225nm), the sample of prochloraz reverse phase high performance liquid chromatography, external standard. You can also use capillary gas Chromatography, chromatographic operating conditions given in Appendix A.

4.3.2 Reagents and solutions

Methanol. HPLC grade;

Acetonitrile. HPLC grade;

Water. The new secondary steam distilled water;

Prochloraz standard. a known mass fraction, >=98.0%.

4.3.3 Instruments

High performance liquid chromatography. a variable wavelength UV detector;

Chromatographic data processor or chromatography workstation;

Column. 250mm × 4.6mm (. I.d) stainless steel column, built AgilentTC-C18,5µm filler (or with equivalent effect Column);

Filter. pore size of about 0.45µm;

Micro injector. 50µL;

Quantitative sample line. 5µL;

Ultrasonic cleaner.

4.3.4 HPLC operating conditions

Mobile phase. psi (methanol. acetonitrile. water) = 30.40.30 by membrane filtration, and degassing;

Flow rate. 1.0mL/min;

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

Detection wavelength. 225nm;

Injection volume. 5µL;

Retention time. about 12.0min.

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 prochloraz EC HPLC is shown in Figure 1.

1 --- prochloraz.

Figure 1 Prochloraz EC HPLC diagram

4.3.5 Measuring step

4.3.5.1 Preparation of standard solution

Weigh 0.1g (accurate to 0.0002g) Prochloraz standard in 50mL volumetric flask, dissolved in methanol and diluted to the mark. use Pipette above solution 10mL in 50mL volumetric flask, diluted with methanol to the mark.

4.3.5.2 Preparation of sample solution

Weigh containing prochloraz 0.1g (accurate to 0.0002g) sample in 50mL volumetric flask, dissolved in methanol and diluted to the mark, shake uniform. Using a pipette to take the above solution 10mL in 50mL volumetric flask, diluted with methanol to the mark.

4.3.5.3 Determination

Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles prochloraz peak area relative change After less than 1.5%, according to the solution, sample solution, sample solution, standard order of standard solution was measured.

4.3.6 Calculation

The two needle sample solution and measured before and after the two doses of the standard sample solution PROCHLORAZ peak areas are averaged. Sample PROCHLORAZ the mass fraction of 1 (%), according to equation (1) calculation; (2) to calculate the concentration of rho1 (g/L), according to the formula.

1 = A2

rho1 =

Where.

A1 --- the average standard solution PROCHLORAZ peak area;

A2 --- sample solution Prochloraz amines mean peak area;

Density rho --- 20 °C when the sample in grams per milliliter (g/mL) (according to GB/T 4472 measured);

--- Prochloraz standard mass fraction, expressed as a percentage.

4.3.7 Allowable difference

Prochloraz mass fraction two parallel determination results relative error should not exceed 2.5%, and the arithmetic mean as a measurement result.

4.4 2,4,6-trichlorophenol mass fraction determination

4.4.1 Method summary

Sample was dissolved in methanol, acetonitrile + water as the mobile phase, to use as filler AgilentTC-C18 stainless steel column and UV detector (215nm), the sample of 2,4,6-trichlorophenol by reverse phase high performance liquid chromatography, external standard.

4.4.2 Reagents and solutions

Acetonitrile. HPLC grade;

Water. The new secondary steam distilled water;

2,4,6-trichlorophenol standard. a known mass fraction >=99.0%.

4.4.3 Instruments

High performance liquid chromatography. a variable wavelength UV detector;

Chromatographic data processor or chromatography workstation;

Column. 250mm × 4.6mm (. I.d) stainless steel column, built AgilentTC-C18,5µm filler (or with equivalent effect Column);

Filter. pore size of about 0.45µm;

Micro injector. 50µL;

Quantitative sample line. 5µL;

Ultrasonic cleaner.

4.4.4 HPLC operating conditions

Mobile phase. psi (acetonitrile. water) = 55.45, by membrane filtration, and degassing;

Flow rate. 1.0mL/min;

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

Detection wavelength. 215nm;

Injection volume. 5µL;

Retention time. about 4.0min.

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 prochloraz EC 2,4,6-trichlorophenol measured by HPLC is shown in Figure 2.

1 --- 2,4,6-trichlorophenol;

2 --- prochloraz.

Figure 2 prochloraz EC 2,4,6-trichlorophenol by high performance liquid chromatogram

4.4.5 Measuring step

4.4.5.1 Preparation of standard solution

Weigh 0.01g (accurate to 0.0002g) 2,4,6- trichlorophenol standard sample in 50mL volumetric flask, dissolved in methanol and diluted to the mark Degree, shake.

4.4.5.2 Preparation of sample solution

Weigh-containing 2,4,6-trichlorophenol 0.01g (accurate to 0.0002g) sample in 50mL volumetric flask, dissolved in methanol and diluted to Mark and shake.

4.4.5.3 Determination

Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles 2,4,6-trichlorophenol peak area After the relative change of less than 1.5%, according to the solution, sample solution, sample solution, standard order of standard solution was measured.

4.4.6 Calculation

The two needle sample solution and measured before and after the two doses of the standard sample solution of 2,4,6-trichlorophenol peak areas are averaged. test Samples 2,4,6-trichlorophenol 2 mass fraction (%), according to equation (3) Calculated.

2 = A2

Where.

A1 --- standard solution of 2,4,6-trichlorophenol mean peak area;

--- The A2 in the sample solution of 2,4,6-trichlorophenol average peak area;

--- 2,4,6-trichlorophenol standard mass fraction, expressed as a percentage.

4.4.7 Allowable difference

The relative deviation of two measurements shall be not more than 20% of the arithmetic mean as a measurement result.

4.5 Determination of Moisture

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

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, the non-oil slick, no precipitation under 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. Thermal storage after prochloraz content should be not less than 95% before the thermal storage, other indicators should Meet the requirements of this standard is qualified.

4.10 Product inspection and acceptance

Shall comply with GB/T 1604's. Limit numerical processing using rounding value comparison method.