GB 22610-2008Carbosulfan granules (English PDF)

4.1 Sampling

In accordance with GB/T 1605-2001 of "solid preparation sampling" approach. Determining Sample packages with a random number table method; Final sample the amount should be less than 600g.

4.2 Identification Test

4.2.1 Liquid Chromatography --- This identification test can be carried out simultaneously with the determination of the mass fraction of carbosulfan. In the same chromatographic operating conditions the lower member, carbosulfan peak of a peak retention time of a sample solution and the standard solution retention time, the relative difference should 1.5% or less.

Determination of the mass fraction of 4.3 carbosulfan (carbofuran)

4.3.1 Method summary

Sample was dissolved in methanol, + water as the mobile phase, used as a filler AgilentTC-C18 stainless steel column and UV detector (280 nm), the sample carbosulfan reverse phase high performance liquid chromatography, external standard.

4.3.2 Reagents and solutions

Methanol. HPLC grade;

Water. The new secondary steam distilled water;

Carbosulfan Sample. A known mass fraction omega>=98.0%;

Carbofuran Sample. A known mass fraction omega>=99.0%;

Carbofuran Preparation of standard solution. Weigh 0.05 g of carbofuran standard (accurate to 0.0002g) was placed in a 50mL volumetric flask, washed with methanol Dissolved and diluted to the mark.

4.3.3 Instruments

HPLC. a variable wavelength UV detector;

Chromatographic data processor or workstation;

Column. 250mm × 4.6mm (. I.d) stainless steel column, built AgilentTC-C18,5µm filler (or with equivalent effect color Spectrum column);

Filter. membrane pore size of about 0.45 m;

Microsyringe. 50µL;

Quantitative sampling tube. 5µL;

Ultrasonic cleaning.

4.3.4 HPLC operating conditions

Mobile phase. [Psi] (methanol. water) = 88.12, by membrane filtration, and degassing;

Flow rate. 1.0mL/min;

Column temperature. room temperature (temperature change should be less than 2 deg.] C);

Detection wavelength. 280nm;

Injection Volume. 5µL;

Retention time. 3.6min carbofuran, carbosulfan 13.8min.

Are typical operating parameters of the above, according to the characteristics of different instruments, for a given operating parameters appropriately adjusted to obtain the best result.

A typical carbosulfan EC shown in Figure 1 HPLC.

1 --- carbofuran;

2 --- carbosulfan.

FIG FIG 1 HPLC carbosulfan granules

4.3.5 Determination Step

4.3.5.1 Preparation of standard solution

Weigh 0.1 g of carbosulfan standard (accurate to 0.0002g), a 50mL volumetric flask, dissolve and dilute to volume with methanol, Shake well. Pipette accurately pipetted solution is placed above another 10mL 50mL volumetric flask, and then another 2mL pipette take g Budweiser standard solution in the same volumetric flask, dilute to volume with methanol, shake.

4.3.5.2 Preparation of sample solution

Weigh containing 0.1 g of carbosulfan (accurate to 0.0002g) sample, placed in a 50mL volumetric flask, dilute to volume with methanol, the 15min shaking to dissolve the sample under ultrasound, shake. Pipette accurately pipetted solution is placed above another 10mL 50mL volumetric flask , Diluted with methanol, shaken with a pore size of 0.45µm membrane filter.

4.3.5.3 Determination

Under the above operating conditions, after the instrument is stable, the number of consecutive doses of the standard solution is injected until the needle carbosulfan two adjacent opposing peak area After the change is less than 1.0%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.

4.3.6 Computing

The two doses of the standard peak area was measured before and after the two needles in the sample solution and a sample carbosulfan (carbofuran peak area) were Averaged. Sample carbosulfan (carbofuran) mass fraction omega1 (%) according to equation (1).

1 = A2

Where.

A1 --- the standard solution, a peak area carbosulfan (carbofuran peak area) is calculated;

A2 --- sample solution, carbosulfan peak area (carbofuran peak area) is calculated;

--- standard samples carbosulfan (carbofuran) mass fraction, expressed in%;

4.3.7 Allows poor

The measurement results of the mass fraction of carbosulfan two parallel should be less than 0.3% carbofuran parallel measurement results twice a mass fraction of Relative deviation should not exceed 40%, and the arithmetic mean average as a measurement result.

Carried out in GB/T 1601.

Determination of particle size 4.5

4.5.1 Instruments

Group standard sieve. consistent with the indicated pore diameter range, and with the chassis and the sieve cover;

Electric shaker. amplitude of 36mm, 240 times/min.

4.5.2 Determination Step

The standard sieve vertically stacked, placed in a small sieve large particle size above a particle size sieve, sieve bottoms receiving pan, accurately weighed 100g sample (nearest 0.1 g of), placed on the top sieve, stamped seal, a good combination of the screen pack is mounted on a shaker, to start oscillating sieve shaker 10min. Then remove the sieve was weighed within a predetermined size range.

4.5.3 Computing

Sample size omega2 (%) according to equation (2).

Where.

4.6 Determination of Failure Rate

4.6.1 Instruments

Standard sieve. aperture and 4.5.1 "standard sieve set" small particle diameter the same screen;

Ball or balls. 15 (7.9mm);

Electric shaker. amplitude of 36mm, 240 times/min.

4.6.2 Determination Step

Accurately weighed sample was measured over 50g of the particle size, the standard screen 15 into filled with steel balls or balls, the sieve is built into the chassis capped, shift Fixed to the shaker after shaking 15min, the accurately weighed sample quality taken disk access (to the nearest 0.1g).

4.6.3 Computing

Shedding sample rate omega3 (%) according to equation (3) is calculated.

Where.

Thermal storage stability test 4.7 According to GB/T 19136 "other agents" performed after hot storage, carbosulfan content should not be less than the measured mass fraction Prestorage 95%, particle size, should meet the standards was still falling.

4.8 Product testing and acceptance

Shall comply with the provisions of GB/T 1604's. Process limit values using rounding value comparison method.