GB 28126-2011Imidacloprid technical material (English PDF)

3.1 Appearance

White to beige powder, without visible foreign matter.

3.2 Technical Specifications

Imidacloprid should also meet the requirements of Table 1.

Table 1 imidacloprid Control Project Index

Item Index

Imidacloprid content /% >= 97.0 Loss on drying /% <= 0.5 the pH range of 5.0 to 8.0 Dimethylformamide insolubles mass fraction a /% <= 0.2 when a normal production, dimethylformamide insolubles content was measured at least once every three months.

Test Method 4

4.1 Sampling

Carried out in GB/T 1605-2001 of "original drug product sampling" approach. Determining Sample packages with a random number table method; final sample size not less than 100g.

4.2 Identification Test

The present liquid chromatography --- identification test can be conducted simultaneously with the determination of the mass fraction of imidacloprid. Chromatography under the same operating conditions, the test Main peaks in the retention time of the sample solution and the standard solution imidacloprid retention time of the peaks, the relative difference should be less than 1.5%.

Infrared spectroscopy --- imidacloprid standard sample and the infrared 4000cm -1 ~ 400cm-1 absorption spectrum range should not significantly the difference. Imidacloprid standard infrared spectra of Figure 1.

FIG 1 imidacloprid standard IR spectrum

4.3 Determination of the content of Imidacloprid

4.3.1 Method summary

Sample dissolved in mobile phase, methanol and water as mobile phase, used as a filler C18 stainless steel column and UV detector wavelength at 260nm, of the sample imidacloprid RP-HPLC separation and determination, external standard.

4.3.2 Reagents and solutions

Methanol. HPLC grade;

Water. The new secondary steam distilled water;

Imidacloprid Sample. A known mass fraction w>=99.0%.

4.3.3 Instruments

HPLC. a variable wavelength UV detector;

Chromatographic data processor or chromatography 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.

4.3.4 HPLC operating conditions

Mobile phase. [Psi] (methanol. water) = 40.60, by membrane filtration, and degassing;

Flow rate. 0.8mL/min;

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

Detection wavelength. 260nm;

Injection Volume. 5µL;

Retention time. imidacloprid 6.0min.

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 HPLC imidacloprid shown in Figure 2.

1 --- imidacloprid.

FIG 2 FIG imidacloprid original drug HPLC

4.3.5 Determination Step

4.3.5.1 Preparation of standard solution

0.1 g of weighed (accurate to 0.0002g) imidacloprid in Sample 100mL volumetric flask, dissolved in methanol and diluted to the mark, ultrasonic 5min shaken to dissolve the sample, cooled to room temperature, shaking. Pipette with a pipette 5mL above solution in 50mL volumetric flask, with the mobile Phase was diluted to the mark.

4.3.5.2 Preparation of sample solution

Containing 0.1 g of imidacloprid was weighed (accurate to 0.0002g) sample in 100mL volumetric flask, dissolved in methanol and diluted to the mark, ultra 5min sonication to dissolve the sample, cooled to room temperature, shaking. Pipette with a pipette 5mL above solution in 50mL volumetric flask, with Mobile phase and dilute to the mark.

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 two adjacent pins relative change in peak area imidacloprid After less than 1.2%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.

4.3.5.4 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 imidacloprid. Imidacloprid sample Mass fraction by formula (1).

w1 = A2

· M1 · w

A1 · m2

Where.

W1 --- imidacloprid sample mass fraction in%;

A2 --- sample solution, imidacloprid average peak area;

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

W --- the mass fraction of imidacloprid standard sample, expressed in%;

A1 --- the standard solution, the average peak area imidacloprid;

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

4.3.6 Allows poor

The difference between the results of two replicates imidacloprid 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 and Appliances

Weighing bottle. diameter 50mm, height 20mm;

Oven. 105 °C ± 2 °C;

Dryer.

4.4.2 Determination Step

The weighing bottle placed in an oven bake IH, then cooled to room temperature in a desiccator, weighed (accurate to 0.0002g). Repeating the above steps Step, until a constant weight weighing bottle. 10g weighed into a weighing bottle in a sample, paving weighed (accurate to 0.0002g). The weighing bottle back into the oven Me, IH bake uncovered, capped, removed and placed in a desiccator was cooled to room temperature, weigh (accurate to 0.0002g). Repeating the above operation, Weighing bottle and the sample until a constant weight.

4.4.3 Computing

Drying loss mass fraction in a sample according to the formula (2).

w2 = m1-m2m × 100

Where.

--- drying loss mass fraction 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 value as a measurement result.

4.5 PH value measured

Carried out in GB/T 1601.

Determination of insoluble material content of the amide methyl two 4.6

4.6.1 Reagents

dimethylformamide.

4.6.2 Instruments

Erlenmeyer flasks. glass with ground joints, 250mL;

Sand core glass crucible. G3;

Oven. 110 °C ± 2 °C.

4.6.3 Determination Step

Sample Weigh 10g (accurate to 0.01g), placed in 250mL Erlenmeyer flask, 60mL of dimethylformamide was added, shaken to all Solution was taken, filtered through a crucible constant weight solution, and then dimethylformamide 60mL conical flask was washed three times, and suction filtered. The crucible set Dried in an oven 30min, then cooled to room temperature and weighed.

Dimethylformamide insolubles fraction of mass (3) is calculated according to the formula.

w3 = m1-m0m × 100

Where.

W3 --- dimethylformamide insolubles content, expressed in%;

After constant weight mass M1 --- crucible and the insolubles in grams (G);

M0 --- crucible mass in grams (G);

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

4.6.4 Allows poor

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

4.7 Product testing and acceptance

Product inspection and acceptance shall comply with GB/T 1604's. Process limit values using rounding value comparison method.

5.1 Marking, labeling, packaging

Flag imidacloprid, labeling and packaging should comply with the provisions of GB 3796. Imidacloprid original medicinal lined iron drum, barrel, net weight Generally 50kg, 100kg or 200kg. Other forms may also be packed according to the requirements of the protocol or order, subject to the provisions of GB 3796.

5.2 Storage

Imidacloprid package airiness, dry place. Storage and transportation, to prevent moisture and sunlight, no food, seed, feed Feed mix, to avoid contact with the skin, eyes, mouth and nose to prevent inhalation.

5.3 Security

This is a moderately toxic pesticides. Are swallowed and inhaled toxic, it can penetrate through the skin. Wear protective goggles and rubber gloves when using this product Necessary to wear protective clothing. After application with soap and rinse with water. Coverage should be immediately sent to hospital for symptomatic treatment.

5.4 Acceptance of

Acceptance of imidacloprid for a month. From the date of delivery, product quality inspection completed within one month, the indicators should be Meet the standards.

Appendix A

(Informative)

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

ISO common name. Imidacloprid CAS Registry Number. 138261-41-3 CIPAC Numeric Code. 582 Chemical name. 1- (6-chloro-3-pyridylmethyl) -N- nitromethylene-imidazol-2-yl-amine Structure.

Empirical formula. C9H10ClN5O2 Molecular weight. 255.7 Biological activity. insecticide Melting point. 144 °C Vapor pressure (20 °C). 4 × 10-7mPa Solubility (20 °C, g/L). water 0.61, 0.68 toluene, methylene chloride 55, 1.2 isopropanol, n-hexane is less than 0.1 Stability follows. pH of 5 to 11 stable, hard to be hydrolyzed.