GB 29380-2012Tetramethrin technical material (English PDF)

3.1 Composition and appearance

This product should tetramethrin production and related impurities, as a white to pale yellow powder-like or small.

3.2 Technical Specifications

Tetramethrin original drug shall comply with the requirements in Table 1.

Table 1 tetramethrin original drug control project indicators

Item Index

Tetramethrin mass fraction /% >= 92.0 Cis-isomer/trans-isomer (20 ± 5)/(80 ± 5) Acidity (H2SO4 basis) /% <= 0.2 Drying loss mass fraction /% <= 0.5 Acetone insoluble mass fraction /% <= 0.2 Test Method 4

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 standard titration solution, in the absence of other requirements specified, and prepared according to GB predetermined calibration/T 601 a. test result 4.3.3 determination performed by the rounding value in comparison 8170-2008 GB/T .

4.2 Sampling

According to GB/T 1605-2001 of "original drug product sampling" method, is determined by random sampling method of the package, a final sample volume should not be Less than 100g.

4.3 Identification Test

Optionally one of the following methods. When it is not determined by a process should then be determined using another method.

GC --- present identification test can be conducted simultaneously with the determination of the mass fraction of tetramethrin. Under the same chromatographic conditions, the sample solution Retention time and peak tetramethrin solution of a standard sample peak retention time of the solution, the relative difference should be less than 1.5%.

Infrared spectroscopy --- tetramethrin standard sample and the infrared in the range of 4000cm-1 ~ 400cm-1 absorption spectrum should be no significant difference. Tetramethrin standard infrared spectra of Figure 1.

1 tetramethrin standard infrared spectrum of FIG.

4.4 Determination of the mass fraction of tetramethrin and cis-trans isomers

4.4.1 Method summary

Sample was dissolved in ethyl acetate, diisooctyl phthalate esters as internal standard, using the DB-210 capillary column and flame ionization detection Detector, tetramethrin of sample and measured by gas chromatography.

4.4.2 Reagents and solutions

Tetramethrin standard. tetramethrin known mass fraction, w>=98.0%;

Diisooctyl phthalate;

Ethyl acetate;

Internal standard solution. Weigh 0.8g of diisooctyl phthalate, in 100mL volumetric flask, dissolved in ethyl acetate, constant volume, Shake well.

4.4.3 Instruments

Gas chromatograph. with a hydrogen flame ionization detector;

Chromatographic data processor or chromatography workstation;

Column. 30m × 0.25mm (id) DB-210 fused Shi Ying column, film thickness 0.25µm.

4.4.4 Chromatographic operating conditions

Temperature. column compartment 240 °C, the gasification chamber 250 °C, the detector chamber 250 °C;

Gas flow rate. carrier gas (N2) 1.6mL/min, hydrogen 30mL/min, air 400mL/min;

Retention time. about internal standard 3.5min, cis tetramethrin about 4.7min, trans tetramethrin about 5.4min.

Gas chromatography operational conditions described above, a typical system operating parameters; instruments according to different characteristics, for a given operating parameter adjusted as appropriate, in order to for best results. Typical gas chromatograph tetramethrin parent drug shown in Figure 2.

1 --- internal standard;

2 --- cis-tetramethrin;

3 --- trans tetramethrin.

Fig 2 GC tetramethrin original drug and the internal standard

4.4.5 Determination Step

4.4.5.1 Preparation of standard solution

Sample Weigh 0.08 g of tetramethrin (accurate to 0.0002g), in 15mL clean, dry vial was stoppered, was added with a pipette accurately Internal standard solution 10mL, shake.

4.4.5.2 Preparation of sample solution

Weigh a sample containing 0.08g of tetramethrin (accurate to 0.0002g), in 15mL clean, dry vial stoppered with and 4.4.5.1 with a pipette in exact 10mL was added to the standard solution, shake.

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 tetramethrin adjacent peak area relative change 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 tetramethrin and internal standard peak areas were averaged. Sample the mass fraction of tetramethrin by formula (1).

w1 = r2 × m1 × wr1 × m2 (1) where.

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

r1 --- standard solution of cis, trans tetramethrin average peak area and the internal standard peak area ratio;

R2 --- cis sample solution, and an average value of the peak area of the internal standard peak area trans tetramethrin ratio;

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

--- M2 tetramethrin mass of sample, grams (G);

W --- tetramethrin standard samples tetramethrin content, expressed in%.

4.4.5.5 Determination of the cis-isomer/trans-isomer

Determination of the mass fraction determination of tetramethrin and cis-isomer/trans-isomer simultaneously.

The proportion of cis isomer/trans-isomer alpha is calculated according to formula (2).

alpha = A1

/ (A1 A2)

A2/(A1 A2)

Where.

A1 --- cis tetramethrin peak area in the sample solution;

A2 --- peak area of sample solution of trans-tetramethrin.

4.4.5.6 Allow poor

Results measured by a differential mass fraction tetramethrin two parallel, should not exceed 1.2%, and the arithmetic mean value as a measurement result.

4.5 Determination of acidity

4.5.1 Reagents and solutions

Ethanol;

Sodium hydroxide standard titration solution. c (NaOH) = 0.01mol/L;

Methyl red. 1g/L ethanol solution;

Bromocresol Green. 1g/L ethanol solution;

Mixed indicator. methyl red ethanol solution of 2mL and 10mL bromocresol green ethanol solution, mix well.

4.5.2 Procedure

2g sample was weighed (accurate to 0.0002g), placed in 250mL Erlenmeyer flask, absolute ethanol was added 50mL, shaking the sample Dissolving; 6 drops of mixed indicator solution was added, with 0.01mol/L sodium hydroxide standard titration solution titration, the solution changed from red to green as the end point;

At the same time as the blank determination.

4.5.3 Computing

Acidity w2 of the sample (in terms H2SO4), according to equation (3) is calculated.

w2 = c ×

(V1-V0) × M

1000m × 100

Where.

--- acidity content w2 of the sample, expressed in%;

C --- sodium hydroxide concentration standard titration solution in units of moles per liter (mol/L);

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

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

--- m sample mass in grams (G);

--- numerical molar mass M sulfuric acid, in units of grams per mole (g/moL), M 12H2SO ÷ 4 êê úú = 49.04.

4.6 Determination of loss on drying

4.6.1 Instruments

Oven. 50 °C ± 2 °C;

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

Dryer.

4.6.2 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).

4.6.3 Computing

The mass fraction of the sample weight loss by drying of formula (4) is calculated.

w3 = m1-m2m × 100

Where.

W3 --- drying loss mass fraction 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).

4.6.4 Allows poor

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

4.7 Determination of acetone insolubles

According to GB/T 19138 carried out.

4.8 Product testing and acceptance

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

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

5.1 Marking, labeling, packaging

Tetramethrin original drug marker, label, package should meet the requirements of GB 3796; tetramethrin original drug application opening drum lined with double plastic Bag, generally barrel net weight 20kg; ordering protocol according to user requirements or other forms of packaging may be employed, subject to GB 3796 Provisions.

5.2 Storage

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

5.3 Security

Tetramethrin low toxicity pyrethroid insecticides, inhalation or contact with toxic average, the FDA should wear protective equipment, after application should Wash with soap. This product is no specific antidote should be swallowed immediately to the hospital for symptomatic treatment.

5.4 Acceptance of

Tetramethrin original drug acceptance period of one month. From the date of delivery, product quality inspection completed within a month, the indicators should be consistent standard requirement.

Appendix A

(Informative)

Other names, structural formulas and physicochemical parameters of the basic tetramethrin Other names, structural formulas and physicochemical parameters of the product substantially tetramethrin active ingredients are as follows.

ISO common name. tetramethrin CAS Registry Number. 7696-12-0 CIPAC Numeric Code. 322 Chemical Name. cyclohex-1-ene-1,2-dicarboxylic acid imino-methyl (RS) -2,2- dimethyl-3- (2-methyl-prop-1-en-yl) cyclopropanecarboxamide ester Structure.

Empirical formula. C19H25NO4 Molecular weight. 331.42 (according to 2007 international relative atomic mass) Biological activity. Insecticides Vapor pressure (20 °C). 4.7 × 10-2Pa Relative density (20 °C). 1.108 Solubility. Insoluble in water, soluble in xylene, toluene, acetone, ethanol and chloroform.

Stability. stable to heat, light and gradually decomposed at, when alkali and acid decomposition.