GB 29385-2012Pyrimethanil technical material (English PDF)

3.1 Appearance

White powder solid, without visible foreign matter and added modifier.

3.2 Technical Specifications

Pyrimethanil original drug should also meet the requirements of Table 1.

Table 1 pyrimethanil original drug control project indicators

Item Index

Pyrimethanil mass fraction /% >= 97.0 Acetone insolubles a /% <= 0.2 Moisture /% <= 0.5 pH range 6.0 to 10.0 when a normal production, the acetone insoluble matter measured at least once every three months.

Test Method 4

Safety Tips. to use this standard shall have practical experience of laboratory work. This standard does not indicate any safety issues. Make with those who have the responsibility to take appropriate safety and health practices and to ensure compliance with the provisions of relevant state laws and regulations.

4.1 General provisions

This standard reagent in the absence of water and other requirements stated, refer to three predetermined analytical reagents and GB/T 6682-2008 of water. The test results performed by determining 4.3.3 rounding value in comparison 8170-2008 GB/T .

4.2 Sampling

Carried out in GB/T 1605-2001 of "original drug product sampling" approach. Determined by sampling a random number table method packages, the amount of the final sample not less than 100g.

4.3 Identification Test

Infrared spectroscopy --- Sample Sample pyrimethanil IR in the range of 4000cm-1 ~ 400cm-1 absorption spectrum should be no significant difference. Pyrimethanil standard infrared spectra of Figure 1.

HPLC --- This identification test can be carried out simultaneously with the determination of the mass fraction of pyrimethanil. In the same chromatographic operating conditions , The peak of a retention time in the sample solution and the standard solution of amine Pyrimethanil retention time, the relative difference should be less than 1.5%.

cm-1

1 pyrimethanil standard infrared spectrum of FIG.

Determination of the mass fraction of 4.4 pyrimethanil

4.4.1 Method summary

Sample dissolved in mobile phase, methanol water, phosphoric acid as the mobile phase, used as a filler C18 stainless steel column and UV detector (300 nm), the sample pyrimethanil reverse phase high performance liquid chromatography, external standard. It may also be determined using gas chromatography, color Spectrum operating conditions, see Appendix B.

4.4.2 Reagents and solutions

Methanol. HPLC grade;

Water. The new secondary steam distilled water;

Phosphoric acid;

Pyrimethanil Sample. pyrimethanil known mass fraction, w>=98.0%.

4.4.3 Instruments

HPLC. a variable wavelength UV detector;

Chromatographic data processor or workstation;

Column. 250mm × 4.6mm (id) stainless steel column, the contents C18,5µm filler;

Filter. membrane pore size of about 0.45 m;

Microsyringe. 50µL;

Quantitative sampling tube. 5µL;

Ultrasonic cleaning.

4.4.4 HPLC operating conditions

Mobile phase. [Psi] [methanol. water (adjusted with phosphoric acid pH = 3)] = 75.25, filtered through a filter, and degassed;

Flow rate. 1.0mL/min;

Column temperature. room temperature;

Detection wavelength. 300nm;

Injection Volume. 5µL;

Retention time. pyrimethanil about 5.5min.

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.

Typical pyrimethanil original drug by HPLC is shown in Figure 2.

1 --- pyrimethanil.

Figure 2 HPLC original drug pyrimethanil

4.4.5 Determination Step

4.4.5.1 Preparation of standard solution

Weigh 0.1 g of pyrimethanil standard (accurate to 0.0001g), was placed in a 50mL volumetric flask, add the mobile phase is shaken to dissolve, with the flow Phase was diluted to the mark. With the above-described pipette 5mL sample solution flows to the other phase in dilute 50mL volumetric flask, Shake well.

4.4.5.2 Preparation of sample solution

Weigh 0.1g pyrimethanil containing sample (nearest 0.0001g), was placed in a 50mL volumetric flask, add the mobile phase is shaken to dissolve, with Mobile phase and dilute to the mark. With the above-described pipette 5mL sample solution flows to the other phase in dilute 50mL volumetric flask, Shake well.

4.4.5.3 Determination

Under the above operating conditions, after the instrument is stable, the number of consecutive doses of the standard solution is injected until the two needles pyrimethanil relative change in peak area adjacent After less than 1.2%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.

4.4.5.4 Computing

The two needle and the sample solution was measured before and after the two doses of the standard sample solution Pyrimethanil average peak area, respectively. Pyrimethanil sample the mass fraction, calculated according to formula (1).

w1 = A2

· M1 · w

A1 · m2

Where.

W1 --- pyrimethanil sample mass fraction in%;

A2 --- sample solution, pyrimethanil average peak area amine;

M1 --- Sample mass in grams (G);

W --- Sample pyrimethanil amine content, expressed in%;

A1 --- the standard solution, pyrimethanil average peak area amine;

--- M2 sample mass, in grams (g).

4.4.5.5 Allow poor

Results difference pyrimethanil replicates should be less than twice the mass fraction of 1.2%, and the arithmetic mean value as a measurement result.

4.5 Determination of acetone insolubles

According to GB/T 19138 carried out.

4.6 Determination of Moisture

According to GB/T 1600 in a "Karl Fischer method."

4.7 PH value measured

Carried out in GB/T 1601.

4.8 Product testing and acceptance

Shall comply with the provisions of GB/T 1604's.

5.1 Marking, labeling, packaging

Flag pyrimethanil original drug, labeling and packaging should comply with the provisions of GB 3796.

Pyrimethanil original drug packaging is lined with plastic bags or cardboard drum barrel (bag) weight 25kg. Also available upon request Agreement or order other forms of packaging, subject to the provisions of GB 3796.

5.2 Storage

Pyrimethanil original drug package airiness, drying, low temperature warehouses. Storage and transportation, to prevent moisture and sunlight, no food, seed Promoter, feed-mixing, avoid contact with the skin, eyes, mouth and nose to prevent inhalation.

5.3 Security

Pyrimethanil fungicide is low toxicity, ingestion and inhalation are toxic, irritating to the eyes, the FDA should wear protective equipment, after application should Wash with soap, once swallowed, should be immediately sent to hospital for symptomatic treatment.

5.4 Acceptance of

Pyrimethanil original drug acceptance period of one month. The quality of the finished product acceptance within one month from the date of delivery, the indicators should be consistent with standard Prospective requirements.

Appendix A

(Informative)

Other names pyrimethanil, and basic physicochemical parameters of the formula Other names, structural formulas and physicochemical parameters of the product basic active ingredient pyrimethanil as follows.

ISO common name. pyrimethanil CAS Registry Number. 53112-28-0 CIPAC Numeric Code. 714 Chemical name. N- (4,6- dimethyl-pyrimidin-2-yl) aniline Structure.

Empirical formula. C12H13N3 Molecular weight.199.25 Biological activity. bactericidal Melting point. 96.3 °C Vapor pressure (25 °C). 2.2 × 10-3Pa Solubility (20 °C, g/L). 0.121 water (pH = 6.1,25 °C), acetone 389, 617 in ethyl acetate, dichloromethane 1000, 23.7 n-hexane, toluene, 412, 176 methanol Stability. The stability in water and pH dependent, stable storage 54 °C 14d.

Appendix B

(Informative)

Pyrimethanil mass fraction of gas chromatographic method B.1 Method summary Samples with chloroform (or dimethylformamide) was dissolved, di-n-butyl phthalate as an internal standard, using HP-5 as filler Capillary column and flame ionization detector, a sample of pyrimethanil and measured by gas chromatography internal standard method.

B.2 reagents and solutions Chloroform (or dimethylformamide);

Pyrimethanil Sample. a known mass fraction, w>=98.0%;

Internal standard. n-butyl phthalate, should not interfere with the analysis of impurities;

Internal standard solution. Weigh di-n-butyl phthalate, 3.5g, was placed 250mL volumetric flask with chloroform (or dimethylformamide) Dissolved and diluted to the mark.

B.3 Instruments

GC. a hydrogen flame ionization detector;

Chromatography or chromatography workstation processor;

Column. 30m × 0.32mm (id) capillary column bonded HP-5 (5% phenyl methyl silicone), film thickness 0.25µm.

B.4 GC operating conditions Temperature. column temperature 180 °C, the gasification chamber 250 °C, the detector chamber 260 °C;

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

Injection volume. 1.0µL;

Retention time. pyrimethanil 3.9min, internal standard 6.3min.

The above-described gas chromatographic operating conditions typical system operating parameters. May be given operating parameters make appropriate adjustments characteristics of different instruments to Obtain the best result. Typical pyrimethanil the drug and internal standard gas chromatography is shown in Figure B.1.

1 --- pyrimethanil;

2 --- internal standard.

Figure B.1 pyrimethanil the drug and internal standard GC FIG.

Measuring step B.5

B.5.1 preparation of standard solution Weigh 0.05 g of pyrimethanil standard (accurate to 0.0001g), was placed in a glass bottle with a stopper, with a pipette 5mL was added to the standard solution, Shake well.

B.5.2 prepared sample solution Weigh a sample contains about 0.05 g of pyrimethanil (accurate to 0.0001g), and placed in a stoppered glass bottle, with a pipette 5mL was added to the standard solution Liquid, shake.

B.5.3 Determination

Under the above operating conditions, the instrument until a stable baseline, the number of consecutive doses of the standard solution is injected, the needle was calculated for each pyrimethanil internal standard peak area when the ratio of repeatability, to be the relative change pyrimethanil two needles internal standard peak area ratio of less than 1.2% is adjacent, in accordance with standard sample solution, the sample Solution, the sample solution and standard solution were sequentially measured.

B.6 computing

The two pins of the sample solution and the two measured doses of the standard solution of pyrimethanil and internal standard peak area ratio of the sample before and after averaging, respectively.

Pyrimethanil sample mass fraction amine according to formula (B.1) is calculated.

w1 = r2

· M1 · w

r1 · m2

Where.

W1 --- pyrimethanil sample mass fraction in%;

R2 --- sample solution, pyrimethanil and average internal standard peak area ratio;

M1 --- Sample mass in grams (G);

W --- Sample pyrimethanil amine content, expressed in%;

R1 --- the standard solution, pyrimethanil and average internal standard peak area ratio;

--- M2 sample mass, in grams (g).

B.7 allow poor

The measurement results of the two parallel error should not exceed 1.2%, and the arithmetic mean value as a measurement result.