GB 28131-2011Deltamethrin technical material (English PDF)

3.1 Appearance

White crystal powder.

3.2 Technical Specifications

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

Table 1 deltamethrin original drug control project indicators

Item Index

Deltamethrin content /% >= 98.5 Drying loss mass fraction /% <= 0.5 the pH range of 4.0 to 7.0 Test Method 4

4.1 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.

4.2 Identification Test

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

Infrared spectroscopy --- deltamethrin standard sample and the infrared in the range of 4000cm-1 ~ 400cm-1 absorption spectrum should ignorance Significant differences. Deltamethrin standard infrared spectra of Figure 1.

FIG 1 deltamethrin standard IR spectrum

4.3 Determination of the content of deltamethrin

4.3.1 Method summary

Sample dissolved in mobile phase, isooctane dioxane as the mobile phase, used as a filler ZorbaxRX-Sil stainless steel column and purple Outer detector (254nm), deltamethrin sample of normal phase high performance liquid chromatography, external standard.

4.3.2 Reagents and solutions

Iso-octane;

Dioxane;

Deltamethrin Sample. deltamethrin known mass fraction w>=99.0%.

4.3.3 Instruments

HPLC. a variable wavelength UV detector;

Chromatographic data processor;

Column. 250mm × 4.6mm (id) stainless steel column, built ZorbaxRX-Sil, 5µm packing;

Filter. membrane pore size of about 0.45 m;

Microsyringe. 50µL;

Quantitative sampling tube. 10µL;

Ultrasonic cleaning.

4.3.4 HPLC operating conditions

Mobile phase. [Psi] (isooctane. dioxane) = 90.10, by membrane filtration, and degassing;

Flow rate. 1.0mL/min;

Column temperature. room temperature;

Detection wavelength. 254nm;

Injection volume. 10µL;

Retention time. deltamethrin about 5.4min.

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.

Deltamethrin typical normal phase HPLC TC shown in Figure 2.

1 --- deltamethrin.

FIG normal phase high performance liquid chromatography of the original drug deltamethrin 2

4.3.5 Determination Step

4.3.5.1 Preparation of standard solution

Sample Weigh 0.05 g of deltamethrin (accurate to 0.0002g), was placed in a 50mL volumetric flask, add the mobile phase is shaken to dissolve, stream the mobile phase was diluted to the mark.

4.3.5.2 Preparation of sample solution

Weigh 0.05g of deltamethrin-containing sample (accurate to 0.0002g), was placed in a 50mL volumetric flask, add the mobile phase solvent shaken so Solution, dilute to the mark with the mobile phase, shake.

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 peak area of the adjacent two pins is relatively deltamethrin After less than 1.2% of, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.

4.3.6 Computing

The two needle and the sample solution was measured before and after the two doses of the standard sample solution and peak areas were averaged deltamethrin. Sample Deltamethrin Permethrin mass fraction according to formula (1).

w1 = A2

· M1 · w

A1 · m2

Where.

W1 --- deltamethrin sample content, expressed in%;

A2 --- sample solution deltamethrin average peak area;

M1 --- deltamethrin standard mass in grams (G);

W --- Sample deltamethrin content, expressed in%;

A1 --- Sample average peak area was deltamethrin;

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

4.3.7 Allows poor

The difference between the results of two replicates deltamethrin content should not exceed 1.2%, and the arithmetic mean value as a measurement result.

Determination of loss on drying 4.4 mass fraction

4.4.1 Instruments

Oven. 80 °C ± 2 °C;

Weighing bottle. an inner diameter of 70mm, 40mm high;

Dryer.

4.4.2 Determination Step

The weighing bottle placed in an oven bake IH, placed in a desiccator taken cooled to room temperature, weigh (accurate to 0.0002g). Repeating the above steps Step, until a constant weight weighing bottle. 2g sample was placed in the bottle, paving, weighed (accurate to 0.01g), the weighing bottle placed in an oven, without After the lid, bake 2h, removed and placed in a desiccator to cool to room temperature, weigh (accurate to 0.0002g).

4.4.3 Computing

Loss on drying of the sample according to the formula (2).

w2 = m1-m2m × 100

Where.

Loss on drying --- w2 of the sample, expressed in%;

M1 --- sample mass before drying and weighing bottles in grams (G);

--- M2 sample mass after drying and weighing bottles in grams (G);

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

4.4.4 Allows poor

The measurement results of the two parallel relative deviation should not exceed 30%; and the arithmetic mean as a measurement result.

4.5 PH value measured

Carried out in GB/T 1601.

4.6 Product testing and acceptance

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

5 marking, labeling, packaging, storage, security and acceptance of

5.1 Marking, labeling, packaging

Flag deltamethrin original drug, labeling and packaging should comply with the provisions of GB 3796; deltamethrin original drug use clean, dry polyurethane Barrel, net content should be less than 200kg; Other forms of packaging can be employed according to user requirements or ordering protocols, subject to the provisions of GB 3796.

5.2 Storage

Deltamethrin original drug package airiness, dry place; storage and transportation, prevent moisture and sunlight, no food, seeds and feed Feed mix, to avoid contact with the skin, eyes, mouth and nose to prevent inhalation.

5.3 Security

Deltamethrin is moderately toxic pyrethroid insecticides, inhalation or contact with all of toxic if swallowed potentially fatal, exposure can cause eye pain, Skin allergies. FDA should wear protective equipment, wash with soap after application. This product is no specific antidote, mainly the elimination of poison Matter and symptomatic treatment.

5.4 Acceptance of

Deltamethrin original drug acceptance period of one month. From the date of delivery, product quality inspection completed within one month, the indicators should break Together standards.

Appendix A

(Informative)

Deltamethrin other names, structural formulas and physicochemical parameters of the basic Other names, structural formulas and physicochemical parameters of the product basic active ingredient deltamethrin follows.

ISO common name. Deltamethrin CIPAC Numeric Code. 333 Chemical name. (S) -alpha- cyano-3-phenoxybenzyl (1R, 3R) -3- (2,2- dibromo-vinyl) -2,2-dimethyl-cyclopropane carboxylate Structure.

Empirical formula. C22H19Br2NO3 Molecular weight. 505.2 Biological activity. Insecticides Melting point (°C). 98 ~ 101 Vapor pressure (25 °C). 2.0 × 10-6Pa Solubility (g/L, 20 °C). water