GB 24751-2009Clomazone technical (English PDF)

3.1 Appearance

Colorless to pale yellow viscous liquid or white to pale yellow solid, semi-solid substance.

3.2 Technical Specifications

Grass Matsubara drugs should also meet the requirements of Table 1.

Table 1 and grass Matsubara drugs control projects index

Item Index

Grass loose mass fraction /% >= 93.0 Acidity (H2SO4 meter) /% <= 0.3 Moisture /% <= 0.5 Acetone insolubles a /% <= 0.2 Insoluble in acetone measured at least once every 3 months a normal production.

Test Method 4

4.1 Sampling

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

4.2 Identification Test

--- The liquid chromatography with different identification test Determination of the mass fraction of loose grass simultaneously. Under the same chromatographic operating conditions, the sample solution to a chromatographic retention time and different standard solution Pine grass chromatographic retention time, the relative difference should be 1.5% Fewer.

Infrared spectroscopy and different specimen ---Grass loose standard in the range 4000cm-1 ~ 400cm-1 infrared absorption spectrum should not significantly the difference. different Grass loose standard infrared spectrum is shown in Figure 1.

1 Yi Cao loose standard infrared spectrum

4.3 Determination of the mass fraction of pine and grass

4.3.1 Method summary

Sample was dissolved in methanol, acetonitrile + water as the mobile phase, to use as filler AgilentTC-C18 stainless steel column and UV detector 236nm wavelength, the sample of the different grass pine reverse phase HPLC separation and determination of external standard.

4.3.2 Reagents and solutions

Methanol. HPLC grade;

Acetonitrile. HPLC grade;

Water. The new secondary steam distilled water;

Grass Song Sample. a known mass fraction, >=98.0%.

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 AgilentTC-C18,5µm 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 (acetonitrile. water) = 50.50, by membrane filtration, and degassing;

Flow rate. 1.0mL/min;

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

Detection wavelength. 236nm;

Injection volume. 5µL;

Retention time. iso

Grass loose about 11.0min.

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 differences

Grass Matsubara drugs HPLC is shown in Figure 2.

1 --- Yi Cao loose.

Figure 2 HPLC and grass Matsubara drugs

4.3.5 Measuring step

4.3.5.1 Preparation of standard solution

Weigh 0.2g (accurate to 0.0002g) and grass loose standard in 50mL volumetric flask, dissolved in methanol and diluted to the mark.

Using a pipette to take the above solution 10mL in 50mL volumetric flask, diluted with methanol to the mark.

4.3.5.2 Preparation of sample solution

Weigh Iso

Grass pine 0.2g (accurate to 0.0002g) sample in 50mL volumetric flask, dissolved in methanol and diluted to the mark, shake uniform. Using a pipette to take the above solution 10mL in 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 iso Peak area becomes relatively loose grass After less than 1.2% of the solution in accordance with the sample solution, the sample solution and standard sequence of the standard solution was measured.

4.3.6 Calculation

The measured before and after the two-needle sample solution and sample two different doses of the standard solution Grass Pine Peak area were averaged. Sample different Grass loose mass fraction of 1 (%), according to equation (1).

1 = A2

Where.

--- Yi Cao Song Sample mass fraction, expressed as a percentage;

A1 --- the standard solution, the average peak area of pine and grass;

A2 --- sample solution, the average peak area of pine and grass;

4.3.7 Allowable difference

Poor quality grass pine fraction of two parallel determination results shall not be greater than 1.5%, the arithmetic mean value as a measurement result.

4.4 Determination of acetone insolubles

According to GB/T 19138 performed.

4.5 Determination of Moisture

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

4.6 Determination of acidity

4.6.1 Reagents and solutions

95% ethanol;

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

Mixed indicator solution. bromocresol green ethanol solution (1g/L) + methyl red ethanol solution (2g/L) = 3 + 1, according to GB/T 603 formulation.

4.6.2 Measuring step

Weigh iso

Pine grass samples 2g (accurate to 0.002g), placed in 250mL flask, add 100mL95% ethanol, 3 drops instructions Solution, titrated with sodium hydroxide standard titration solution to green, do not fade in the 30s for the end. Make a blank test simultaneously.

4.6.3 Calculation

2 sample acidity (%), according to equation (2).

Ba 1- Vp Vp = 2 () 0

100 (2)

Where.

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

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

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

--- The M values of the molar mass of sulfuric acid, in units of grams per mole (g/mol) M 12H2SO () 4 [] = 49.

4.7 Product testing and acceptance

Product inspection and acceptance shall comply with GB/T 1604's. Treatment of extreme values using the rounding value comparison method.