GB 22171-200815% paclobutrazol wettable powders (English PDF)

4.1 Sampling

According to GB/T 1605-2001 "on solid preparation sampling" approach. Determining sample package using a random number table method; the final sample size not less than 300g.

4.2 Identification Test

Liquid chromatography --- The identification test can be carried out simultaneously with the determination of MET Quality Score. Under the same chromatographic operating conditions, the test the retention time of the sample solution and the standard solution to a peak in the MET peak retention time, the relative difference should be less than 1.5%.

Gas Chromatography --- The identification test can be carried out simultaneously with the determination of MET Quality Score. Under the same chromatographic operating conditions, the test the retention time of the sample solution and the standard solution to a peak in the MET peak retention time, the relative difference should be less than 1.5%.

Determination of the mass fraction of 4.3 MET

4.3.1 Liquid Chromatography (Arbitration Act)

4.3.1.1 Method summary

Sample was dissolved in methanol, - acetonitrile - water as mobile phase, the choice of Nova-pakC18,5µm stuffing column and UV variable Wavelength detector to sample the MET liquid chromatography separation and determination.

4.3.1.2 Reagents and solutions

Methanol. HPLC grade;

Acetonitrile. chromatographic pure;

Water. The new secondary steam distilled water;

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

4.3.1.3 Instruments

LC. a variable wavelength UV detector and quantitative injection valve;

Chromatographic data processor or chromatography workstation;

Column. 3.9mm (i.d.) × 150mm stainless steel columns, built-Nova-pakC18,5µm filler (or with the same column efficiency Other reversed phase columns);

Ultrasonic bath;

Filter. pore size of about 0.45µm;

Micro Injector. not less than 50µL.

4.3.1.4 LC operating conditions

Mobile phase. psi (CH3OH.CH3CN.H2O) = 35.20.45;

The mobile phase flow rate. 1.0mL/min;

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

Detection wavelength. 230nm;

Injection volume. 10µL;

Retention time (min). 4-H 3.8 MET, MET II body 6.3, 7.7 MET, chlorine trazodone 9.6.

HPLC operating conditions described above, the Department of typical operating parameters. According to the characteristics of different instruments, given operating parameters adjusted as appropriate, in order to obtain the best results. Typical liquid chromatograph Paclobutrazol 15% wettable powder shown in Figure 1.

1 --- 4-H MET;

2 --- MET II body;

3 --- MET;

4 --- chlorine trazodone.

Figure 1 LC 15% Paclobutrazol wettable powder

4.3.1.5 Measurement procedure

4.3.1.5.1 Preparation of standard solution

Weigh MET standard 0.10g (accurate to 0.0002g), a 50mL volumetric flask, add 40mL of methanol, in an ultrasonic Bath sonication 5min. Remove cooled to room temperature, add methanol to volume, shake; pipette imbibe 5mL, set another 50mL volumetric flask, add methanol to volume, shake.

4.3.1.5.2 Preparation of the sample solution

Weigh the sample 0.07g (accurate to 0.0002g), a 50mL volumetric flask, add 40mL of methanol, in an ultrasonic bath Sonication 5min. Removed, cooled to room temperature, add methanol to volume, shake; filtered through a membrane filter pore size of about 0.45µm.

4.3.1.5.3 Determination

Under the above chromatographic operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles MET relative peak area After the change is less than 1.0%, according to the order of the standard solution, sample solution, sample solution, standard solution injection analysis.

4.3.1.6 Calculation

The two needle sample solution measured before and after the peak area of the sample and two doses of the standard solution MET are averaged. Sample pleiotropic Azole mass fraction of 1 (%) according to equation (1).

Where.

A1 --- the average peak area of standard solution MET;

The average peak area A2 --- MET in the sample solution;

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

4.3.1.7 Allowable difference

The difference between two parallel determination results shall not be greater than 0.5%, the arithmetic mean value as a measurement result.

4.3.2 Gas Chromatography

4.3.2.1 Method summary

Sample was dissolved in chloroform to triphenylmethane as the internal standard, using a HP-5 (5% + 95% diphenyl dimethyl polysiloxane) painted walls Quartz capillary column and flame ionization detector to sample the MET gas chromatography separation and determination.

4.3.2.2 Reagents and solutions

Chloroform;

Triphenylmethane. Do not interfere with the analysis of impurities;

Internal standard solution. Weigh 5.8g triphenylmethane, in 1000mL volumetric flask with chloroform dissolved and diluted to scale, shake;

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

4.3.2.3 Instruments

Gas chromatograph. with a hydrogen flame ionization detector;

Column. 30m × 0.32mm (i.d.) Quartz capillary column, wall coated HP-5 (5% diphenyl + 95% dimethyl polysiloxane), membrane Thick 0.25µm;

Chromatographic data processor or chromatography workstation.

4.3.2.4 GC operating conditions

Column compartment temperature (temperature programming). initial 200 °C, holding 8min; then to 20 °C/min temperature is increased up to 250 °C, 7min maintained;

Gasification chamber temperature. 280 °C;

Detector temperature. 280 °C;

Gas flow rate (mL/min). carrier gas (N2) 2.0, hydrogen gas 30, air 300, the compensation gas (N2) 25;

Split ratio. 40.1;

Injection volume (µL). 1.0;

Retention time (min). internal standard 5.0, chlorine trazodone 5.6, 6.9 MET, MET MET II body 7.3,4-H 15.1.

GC operating conditions described above, the Department of typical operating parameters. According to the characteristics of different instruments, given operating parameters adjusted as appropriate, in order to obtain the best results. A typical gas chromatogram of 15% Paclobutrazol wettable powder shown in Figure 2.

1 --- internal standard;

2 --- chlorine trazodone;

3 --- MET;

4 --- MET II body;

5 --- 4-H MET.

Figure 2 Gas chromatogram MET 15% wettable powder

4.3.2.5 Measurement procedure

4.3.2.5.1 Preparation of standard solution

Weigh MET standard 0.10g (accurate to 0.0002g), was placed in a 15mL stoppered glass bottle with a pipette accurately added 10mL internal standard solution, dissolve, shake.

4.3.2.5.2 Preparation of the sample solution

Weigh the sample 0.67g (accurate to 0.0002g), was placed in a 15mL stoppered glass vial with 4.3.2.5.1 and with a pipette Accurate internal standard solution was added 10mL dissolved, shake.

4.3.2.5.3 Determination

Under these operating conditions, the instrument until a stable baseline, the number of continuous injection doses of the standard solution, calculate the MET needle and the internal standard peak area Repeatability than when the relative changes in the MET standard peak area ratio of less than 1.2%, according to the standard solution, sample solution to be two adjacent needles, the sample solution, the order of the standard solution was measured.

4.3.2.6 Calculation

The two needle sample solution and measured before and after the two doses of the standard sample solution MET and the internal standard peak area ratios were averaged. test MET sample mass fraction of 1 (%) according to equation (2).

1 = gamma2

Where.

gamma1 --- standard solution, MET and the internal standard peak area ratio of the average;

gamma2 --- sample solution, MET and the internal standard peak area ratio of the average;

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

4.3.2.7 Allowable difference

Twice the difference between the results of the mass fraction of MET parallel determination, should be less than 0.5%, the arithmetic mean value as a measurement result.

4.4 Determination of the suspension rate

4.4.1 Liquid Chromatography (Arbitration Act)

4.4.1.1 Measurement procedure

According to GB/T 14825 performed. Weigh 1.0g sample (accurate to 0.0002g). The cylinder with 60mL methanol remaining 25mL Suspension and precipitate all transferred to 100mL volumetric flask, ultrasonic oscillating 5min, cooled to room temperature, methanol was added to volume, Shake; filtered through a membrane filter pore size of about 0.45µm. 4.3.1 Determination of which MET quality.

4.4.1.2 Calculation

Suspension rate 2 (%) calculation formula shown below.

111.1 (3)

Where.

A1 --- the average peak area of standard solution MET;

A2 --- the average peak area of MET by the remaining 25mL sample solution and precipitate suspension formulated in;

1 --- MET sample mass fraction, expressed as a percentage;

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

4.4.1.3 Allowable difference

The difference between two parallel determination results shall not be greater than 5% of the arithmetic mean as a measurement result.

4.4.2 Gas Chromatography

4.4.2.1 Measurement procedure

According to GB/T 14825 performed. Weigh 1.0g sample (accurate to 0.0002g). With 60mL of water remaining in the cylinder of 25mL Suspension and precipitate all transferred to 100mL beaker. After drying the beaker on the 100 °C ± 2 °C oven or boiling water bath, and 4.3.2.5.1 pipette with an accurate internal standard solution was added 10mL dissolved, shake. 4.3.2 Determination by which MET quality.

4.4.2.2 Calculation

Suspension rate 2 (%) is calculated as follows.

111.1 (6)

Where.

gamma1 --- standard solution, MET and the internal standard peak area ratio of the average;

gamma2 --- by the remaining 25mL sample solution and precipitate suspension formulated after drying, the MET and the internal standard peak area ratio average value;

1 --- MET sample mass fraction, expressed as a percentage;

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

4.4.2.3 Allowable difference

The difference between two parallel determination results shall not be greater than 5% of the arithmetic mean as a measurement result.

4.5 Determination of Moisture

According to GB/T 1600 in the "azeotropic distillation method".

According to GB/T 1601 carried out.

4.7 Determination of wetting time

According to GB/T 5451 carried out.

4.8 Fineness

According to GB/T 16150 in the "wet sieve method".

4.9 Thermal storage stability test

According to GB/T 19136 in "powder formulations" to. MET after the heat storage mass fraction, the suspension was still in line with the requirements for qualified 3.2.

4.10 Product inspection and acceptance

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