GB 9557-2008phoxim emulsifiable concentrates (English PDF)

3.1 Composition and appearance

This product should be compliant phoxim the original drug is made of a homogeneous oily liquid, may appear a little precipitate after storage.

3.2 Technical Specifications

40% phoxim EC shall comply with the requirements of Table 1.

Table 1 40% phoxim EC Control Project Index

Item Index

Phoxim mass fraction (in cis phoxim meter) /% >= 40.0 Moisture /% <= 0.5 Acidity (H2SO4 meter) /% <= 0.3 Emulsion stability (diluted 200 times) Qualified Low temperature stability a qualified Thermal storage stability of a qualified a low temperature stability test, the thermal storage stability tests at normal production, at least every three months, once detected.

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 phoxim content. Under the same chromatographic operating conditions, the test A sample solution peak retention time compared with standard sample solution cis phoxim chromatographic retention time, the relative difference should be 1.5% Fewer.

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.

A typical 40% phoxim HPLC is shown in Figure 1.

1 --- cis phoxim.

Figure 1 40% phoxim EC HPLC 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 0.8%, 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;

Methyl red ethanol solution. rho (methyl red) of 1g/L;

Bromocresol green ethanol solution. rho (bromocresol green) to 1g/L;

Mixed indicator. psi (methyl red ethanol solution. bromocresol green ethanol solution) = 5.

4.5.2 Measuring step

Weigh the sample 5g (accurate to 0.0002g), placed in a 250mL Erlenmeyer flask, add 95% ethanol 50mL, shake the sample Dissolved. Added 2mL mixed indicator, titrated with sodium hydroxide standard titration solution, the solution changes from red to green is shallow end. Simultaneously Blank determination.

4.5.3 Calculation

Acidity 2 (%) of the sample, according to equation (2).

Ba 2 =

(Vp Vp 1- 0) · M

100 (2)

Where.

Ba --- the actual concentration of sodium hydroxide standard titration solution, expressed in moles per liter (mol/L);

Vp 1 --- titration of the sample solution, the volume of consumption of sodium hydroxide standard titration solution, in milliliters (mL);

V0 --- titrate blank solution, the volume of consumption of sodium hydroxide standard titration solution, in milliliters (mL);

--- The M values of the molar mass of sulfuric acid, in units of grams per mole (g/mol), [M (1/2H2SO4) = 49g/mol].

4.6 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.

4.7 Low temperature stability test

According to GB/T 19137 in "liquid preparation", in the bottom of the centrifuge tube educt volume does not exceed 0.3mL qualified.

4.8 Thermal storage stability test

According to GB/T 19136 in "liquid formulation" to. After the thermal storage, mass fraction of 40% phoxim should not be less than the measured mass fraction before hot storage 90%, not more than 0.4% acidity, emulsion stability should continue to meet the standards.

4.9 Product testing and acceptance

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