GB 24756-2009Buprofezin technical (English PDF)

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

Infrared spectroscopy --- sample and standard samples in the IR 4000cm-1 ~ 400cm-1 Scope absorption spectrum should be no significant difference. Thiophene Piperazinone standard infrared spectrum is shown in Figure 1.

Figure 1 buprofenzin standard infrared spectrum

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

4.3 Buprofenzin mass fraction determination

4.3.1 Method summary

Sample was dissolved in chloroform, dicyclohexyl phthalate esters as internal standard, using the 5% HP-5 capillary column coated walls and hydrogen Flame ionization detector, the sample of buprofezin gas chromatography separation and determination. You can also use packed column gas chromatography, strip Member See Appendix A.

4.3.2 Reagents and solutions

Chloroform;

Buprofenzin standard. a known mass fraction, >=98.0%;

Dicyclohexyl phthalate esters. interference analysis should not contain impurities;

Internal standard solution. Weigh 4.0g dicyclohexyl phthalate esters, placed in 500mL flask with chloroform dissolved and diluted to the mark Degree, shake.

4.3.3 Instruments

Gas chromatograph. with a hydrogen flame ionization detector;

Chromatographic data processor or chromatography workstation;

Column. 30m × 0.32mm (i.d.) Capillary column, wall coated HP-5 (5% + 95% diphenyl dimethyl silicone), the film thickness 0.25µm;

Micro injector. 10µL.

4.3.4 GC operating conditions

Temperature (°C). 230 column temperature, the gasification chamber 270, the detector chamber 280;

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

Split ratio. 20.1;

Injection volume (µL). 1.0;

Retention time (min). 3.8 buprofezin, internal standard 7.0.

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. Typical buprofenzin original drug capillary column gas chromatography is shown in Figure 2.

1 --- solvent;

2 --- buprofezin;

3 --- internal standard (phthalate, dicyclohexyl phthalate).

Figure 2 buprofenzin original drug and the internal standard capillary column gas chromatogram

4.3.5 Measuring step

4.3.5.1 Preparation of standard solution

Weigh buprofenzin standard 0.08g (accurate to 0.0002g) in 15mL stoppered glass bottle with a pipette accurately added 10mL within Standard solution, shake.

4.3.5.2 Preparation of the sample solution

Weigh containing buprofezin 0.08g (accurate to 0.0002g) sample in 15mL stoppered glass bottle with a pipette and 4.3.5.1 with Tube accurately added internal standard solution 10mL, shake.

4.3.5.3 Determination

Under these operating conditions, the instrument until a stable baseline, the number of continuous injection doses of the standard solution until the two needles buprofezin and the internal standard peak adjacent when the area ratio changes by less than 1.2%, according to the solution, the sample solution, the sample solution and standard sequence of the 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 piperazinone and thiophene internal standard peak area ratios are averaged. test 1 sample mass fraction (%) of buprofezin according to formula (1).

Where.

--- Standard samples buprofezin mass fraction, expressed as a percentage.

4.3.7 Allowable difference

Thiophene-one hydrochloride poor quality score measurement results of two parallel, should not exceed 1.2%, and the arithmetic mean as a measurement result.

4.4 Determination of loss on drying

4.4.1 Instruments

Weighing bottle. diameter 50mm, height 20mm;

Oven. 100 °C ± 2 °C;

Dryer.

4.4.2 Measuring step

Bake bottle weighed into 100 °C ± 2 °C oven for 30min, and then into the dryer to cool to room temperature, weigh (to the nearest 0.0002g). In weighing bottle was weighed into a 10g sample (paved weighed accurate to 0.0002g). The weighing bottle placed in an oven, uncovered at 100 °C ± 2 °C bake 1.5h, removed into the drier cooled to room temperature until constant weight was weighed (accurate to 0.0002g).

2 Loss on drying (%) according to equation (2).

100 (2)

Where.

4.5 Determination of acidity or alkalinity

4.5.1 Reagents and solutions

acetone;

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

Hydrochloric acid standard titration solution. Ba (HCl) = 0.02mol/L, according to GB/T 601 preparation and calibration;

Methyl red solution. 1g/L ethanol solution, according to GB/T 603 preparation;

Bromocresol green solution. 1g/L ethanol solution, according to GB/T 603 preparation;

Mixed indicator solution. a solution of methyl red + bromocresol green solution = 2 + 10.

4.5.2 Measuring step

Weigh 2g sample (accurate to 0.0002g) in 250mL conical flask, 50mL acetone solution of mixed indicator solution 5 drops ~ 6 drops of sodium hydroxide standard titration solution was titrated to green as the end point, at the same time make a blank measurement. If the test solution is alkaline, hydrochloric acid required standard Titration solution was titrated to a pink end at the same time make a blank measurement. 3 acidity (%) of the sample according to equation (3) to calculate or alkalinity 4 (%) by (4) Calculation Formula.

3 = Ba

· (Vp Vp 1- 0) · M

100 (3)

Where.

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

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

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

--- The M sulfuric acid molar mass values, in units of grams per mole (g/mol) [M (12H2SO4 ) = 49].

4 = Ba '

· (Vp '1- Vp' 0) · M 100 (4) where.

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

Vp '0 --- titrate blank solution, hydrochloric acid standard titration solution consumption volume in milliliters (mL);

Vp '1 --- titration of the sample solution, hydrochloric acid standard titration solution consumption volume in milliliters (mL);

--- NaOH molar mass of the M values, in units of grams per mole (g/mol) [M (NaOH) = 40].

4.6 Determination of acetone insolubles

According to GB/T 19138 performed.

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.