GB 9556-2008phoxim technical (English PDF)

3.1 Appearance

Pale yellow to reddish brown oily liquid.

3.2 Technical Specifications

Phoxim the original drug should also meet the requirements of Table 1.

Table 1 phoxim the original drug control project indicators

Item Index

Phoxim mass fraction (in cis phoxim meter) /% >= 90.0 Moisture /% <= 0.5 Acidity (H2SO4 meter) /% <= 0.3 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 phoxim content. Under the same chromatographic operating conditions, the test A sample solution peak retention time compared with standard sample solution cis phoxim retention time, the relative difference should be less than 1.5%.

4.3 Determination of the mass fraction of phoxim

4.3.1 Method summary

Sample was dissolved in methanol, + water as the mobile phase, to use as filler Capcel-PakC18 stainless steel column and UV detector (254nm), the sample of phoxim reverse phase high performance liquid chromatography, external standard.

4.3.2 Reagents and solutions

Methanol. HPLC grade;

Water. The new secondary steam distilled water;

Phoxim standard. a known mass fraction >=99.0%.

4.3.3 Instruments

High performance liquid chromatography. a variable wavelength UV detector;

Chromatographic data processor;

Column. 150mm × 4.6mm (. I.d) stainless steel column, built Capcel-PakC18,5µm 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. water) = 75.25, by membrane filtration, and degassing;

Flow rate. 1.0mL/min;

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

Detection wavelength. 254nm;

Injection volume. 5µL;

Retention time. 8.6min.

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 phoxim the original drug HPLC is shown in Figure 1.

1 --- cis phoxim.

Figure 1 phoxim the original drug by high performance liquid chromatogram

4.3.5 Measuring step

4.3.5.1 Preparation of standard solution

Weigh 0.1g phoxim standard (accurate to 0.0002g), a 50mL volumetric flask, dissolved in methanol and diluted to the mark, shake uniform. Using a pipette to take the above solution 5mL to 50mL volumetric flask, dilute with mobile phase to the mark.

4.3.5.2 Preparation of sample solution

Weigh phoxim containing 0.1g sample (accurate to 0.0002g), a 50mL volumetric flask, dissolved in methanol and diluted to the mark, Shake well. Using a pipette to take the above solution 5mL to 50mL volumetric flask, dilute with mobile phase 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 phoxim 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 phoxim peak areas are averaged. Sample phoxim the mass fraction of 1 (%), according to equation (1).

1 = A2

Where.

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

A2 --- sample solution, phoxim mean peak area;

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

4.3.7 Allowable difference

Phoxim poor quality score of 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 the "Karl Fischer method".

4.5 Determination of acidity

4.5.1 Reagents and solutions

95% ethanol;

Sodium hydroxide standard titration solution Ba (NaOH) = 0.02mol/L, according to GB/T 601 preparation and calibration;