GB 22175-2008Diniconazole technical (English PDF)

4.1 Sampling

Carried out according to GB/T 1605 "Product of the original drug sampling" method. Determined by sampling a random number table method packages, the final sample size should be a lot of at 100g.

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%.

Infrared spectroscopy --- sample and standard samples in the infrared range 4000cm-1 ~ 400cm-1 absorption spectrum should be no significant differences (see FIG. 1)

Figure 1 diniconazole standard infrared spectrum

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-C185µm 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. (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 original drug HPLC is shown in Figure 2.

1 --- Diniconazole isomer;

2 --- diniconazole.

Figure 2 diniconazole original drug 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.

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 1.2%, the arithmetic mean value as a measurement result.

4.4 Determination of Moisture

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

According to GB/T 1601 carried out.

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