GB 22167-2008Fomesafen technical (English PDF)

3.1 Appearance

This product should be an off-white powder, free from visible foreign matter.

3.2 Technical Specifications

Fomesafen original drug should meet the requirements of Table 1.

Table 1 fomesafen original drug control project indicators

Item Index

Fomesafen mass fraction /% >= 95.0 Acetone insolubles a /% <= 0.5 Loss on drying /% <= 1.0 pH range 3.5 to 6.0 when a normal production, insoluble in acetone at least every three months, once measured.

Test Method 4

4.1 Sampling

According to GB/T 1605-2001 "on the original drug sampling" approach. Determining sample package using a random number table method; the final sample size should not be Less than 100g.

4.2 Identification Test

HPLC --- The identification test can be carried out simultaneously with the determination of the content of fomesafen. In the same chromatographic operating conditions , The sample solution to a chromatographic retention time and standard solution fomesafen chromatographic retention time, the relative difference should 1.5% or less.

Infrared spectroscopy --- sample and standard samples in the infrared range 4000cm-1 ~ 400cm-1 absorption spectrum should be no significant difference, see

Figure 1.

1 fomesafen standard sample infrared spectra in Fig.

4.3 Determination of fomesafen mass fraction

4.3.1 Method summary

Sample was dissolved in methanol, + water + phosphoric acid as the mobile phase, to use as filler HypersilODS stainless steel column and ultraviolet detection Detector (230nm), the sample of fomesafen reverse phase high performance liquid chromatography, external standard.

4.3.2 Reagents and solutions

Methanol. HPLC grade;

Phosphoric acid;

Water. The new secondary steam distilled water;

Fomesafen Sample. Known fomesafen mass fraction >=98.0%.

4.3.3 Instruments

High performance liquid chromatography. a variable wavelength UV detector;

Chromatographic data processor;

Column.200mm × 4.6mm (. I.d) stainless steel column, built HypersilODS, 5µm filler (or with equivalent effect color the 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. water. phosphoric acid) = 600.400.0.2, filtered through a filter membrane and degassed;

Flow rate. 1.0mL/min;

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

Detection wavelength. 230nm;

Injection volume. 5µL;

Retention time. fomesafen 7.8min.

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 fomesafen original drug HPLC is shown in Figure 2.

1 --- fomesafen.

Figure 2 HPLC fomesafen original drug

4.3.5 Measuring step

4.3.5.1 Preparation of standard solution

Weigh fomesafen standard 0.1g (accurate to 0.0002g), a 50mL volumetric flask, dissolved in methanol and diluted to the mark, Shake well. Pipette accurately pipette 5mL above solution was placed in another 50mL volumetric flask, diluted with methanol to the mark.

4.3.5.2 Preparation of sample solution

Weigh fluorine fomesafen 0.1g (accurate to 0.0002g) sample, placed in 50mL volumetric flask, dissolved in methanol and diluted to the mark Degree, shake. Pipette accurately pipette 5mL above solution was placed in another 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 fomesafen relative peak area After the change is less than 1.0%, according to the solution, the sample solution, the sample solution and standard sequence of the standard solution was measured.

4.3.6 Calculation

The two needle sample solution measured before and after the peak area of the sample and two doses of the standard solution of fomesafen were averaged. Specimen Fomesafen mass fraction of 1 (%) according to equation (1).

1 = A2

Where.

A1 --- the standard solution, the average fomesafen peak area;

A2 --- sample solution, the average fomesafen peak area;

--- Standard samples fomesafen mass fraction, expressed as a percentage.

4.3.7 Allowable difference

Determination of fomesafen parallel mass fraction of the difference between the two results should not exceed 1.0%, and the arithmetic mean as a measurement result.

4.4 Determination of acetone insolubles

According to GB/T 19138 Determination.

4.5 Determination of loss on drying

4.5.1 Instruments

Oven. 105 °C ± 2 °C;

Weighing bottle. diameter 70mm, height 40mm;

Dryer.

4.5.2 Measuring step

The weighing bottle placed in an oven bake 1h, was brought out in a desiccator to cool to room temperature, weigh (accurate to 0.0002g). Repeat the above steps Step, until constant weight weighing bottle. 10g sample is placed in the bottle, paving, weighed (accurate to 0.01g), the weighing bottle placed in an oven, without Cover and bake 1h, remove and put in the dryer to cool to room temperature, weighed (accurate to 0.0002g).

4.5.3 Calculation

Loss on drying of the sample mass fraction 2 (%), according to equation (2).

Where.

4.5.4 Allowable difference

The relative deviation of two parallel determination results shall not be greater than ± 15%; the arithmetic mean value as a measurement result.

According to GB/T 1601 Determination.

4.7 Product testing and acceptance

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