GB 22174-2008diniconazole wettable power (English PDF)

4.1 Sampling

Carried out according to GB/T 1605 "solid preparation sampling" method. Determining sample package by random sampling method, the final sample size should not be Less than 300g.

4.2 Identification Test

HPLC --- The identification test with diniconazole determination simultaneously. Under the same chromatographic operating conditions, the sample One solution peak retention time compared with standard sample solution diniconazole chromatographic retention time, the relative difference should be less than 1.5%.

When using the above method for identification of effective ingredients have questions, other effective methods can be used for identification.

4.3 Determination of the mass fraction of diniconazole

4.3.1 Method summary

Sample dissolved in mobile phase, methanol + water as the mobile phase, use as filler to C18 stainless steel column and UV detector (250nm), Other than the standard method of sample diniconazole reverse phase HPLC separation and determination.

4.3.2 Reagents and solutions

Methanol. HPLC grade;

Water. The new secondary steam distilled water;

Diniconazole standards. a known mass fraction >=99.0%.

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 ZORBAXSB-C18,5µm filler (or other equivalent effect Column);

Filter. pore size of about 0.45µm;

Micro injector. 50µL;

Ultrasonic cleaner.

4.3.4 HPLC operating conditions

Mobile phase. psi (methanol. water) = 85.15, by membrane filtration, and degassing;

The mobile phase flow rate. 1.0mL/min;

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

Detection wavelength. 250nm;

Injection volume. 5µL;

Retention time. Diniconazole about 5.6min, diniconazole isomers about 4.5min.

It said operating parameters are typical, according to the characteristics of different instruments and columns for a given operating parameters adjusted as appropriate, in order to obtain the most Good effect. Typical diniconazole WP HPLC is shown in Figure 1.

1 --- Diniconazole isomer;

2 --- diniconazole.

Figure 1 diniconazole WP HPLC chromatogram

4.3.5 Measuring step

4.3.5.1 Sample solution preparation

Weigh diniconazole standards 0.05g (accurate to 0.0002g), placed in 100mL volumetric flask, dissolved in mobile phase and dilute to the mark, Shake well.

4.3.5.2 Sample solution preparation

Weigh the sample containing diniconazole 0.05g of (accurate to 0.0002g), placed in 100mL volumetric flask, dissolved in mobile phase and dilute to Mark and shake. Through 0.45µm membrane filter and set aside.

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 diniconazole 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

Before and after the two-pin solution and the sample solution in the sample measured two doses of the standard solution diniconazole peak areas are averaged. Sample ene Yl alcohol content of 1 (%) according to equation (1).

1 = A2

Where.

Two doses of the standard solution A1 --- alcohol before and after diniconazole mean peak area;

Sample solution before and after the two-pin A2 --- diniconazole mean ol peak area;

--- Standard Diniconazole mass fraction, expressed as a percentage.

4.3.7 Allowable difference

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

4.4 Determination of the suspension rate

4.4.1 Measuring step

According to GB/T 14825 in a method carried out. He said sample of about 1.0g (accurate to 0.0002g), with the amount of 70mL of methanol will remain in the bucket 1/10 suspensions and the residue is transferred to the bottom of the 100mL flask, thoroughly shaken, methanol sonication, set the volume. According to the standard 4.3 Determination diniconazole quality, calculate the suspension rate.

4.4.2 Calculation

Sample 2 was suspended rate (%) according to equation (2).

100 (2)

Where.

4.4.3 Allowable difference

The difference between two parallel determination results shall not be greater than 5% of the arithmetic mean as a measurement result.

4.5 Determination of Moisture

According to GB/T 1600 "on azeotropic distillation method".

According to GB/T 1601 carried out.

4.7 Determination of wetting time

According to GB/T 5451 carried out.

4.8 Determination of fineness

According to GB/T 16150 in the "wet sieve method".

4.9 Thermal storage stability test

19136 by method GB/T "powder formulation" will be completed testing diniconazole mass fraction and suspension rates within 24h after the heat storage set. Diniconazole content should not be less than the reservoir before the mass fraction of 95%, was still suspended shall meet the standards.

4.10 Product inspection and acceptance

Shall comply with GB/T 1604's. Treatment of extreme values using GB/T 1250 rounding value comparison method.