GB 24330-2009General security technical specification for domestic sanitary insecticide (English PDF)

4.1 Requirements for use of active ingredient

It shall be the medicament that is registered for use in accordance with relevant national regulations.

4.2 Toxicology

It shall meet the toxicological test requirements of the corresponding dosage form in the Order of the Ministry of Agriculture and Rural Affairs of the People’s

Republic of China [2007] (No.10).

4.3 Active ingredient content and allowable fluctuation range

4.3.1 The content of active ingredients shall be clearly stated on the product packaging.

4.3.2 The allowable fluctuation range of active ingredient content is shown in

Table 1 and the following regulations.

a) For mosquito coil, cockroach, fly incense and other tobacco preparation products, the allowable fluctuation range of its active ingredient content shall not be higher than 40% of the indicated value and not lower than 20% of the indicated value;

b) For electrothermal mosquito liquid incense, the allowable fluctuation range of its active ingredient content shall not be higher than 25% of the indicated value and not lower than 10% of the indicated value;

c) Electrothermal mosquito tablet incense shall be marked (mg/piece). The

5.3 Active ingredient content and allowable fluctuation range

5.3.1 Visual inspection.

5.3.2 The content of active ingredients shall be tested in accordance with the provisions of Annex A, Annex B, Annex C, and Annex D (unlisted dosage form products shall be implemented according to the test methods in relevant national standards).

5.4 Efficacy

5.4.1 Sprays, aerosols, small aerosols, mosquito coils, electrothermal mosquito

tablet incenses, electrothermal mosquito liquid incenses, cockroach poison baits shall be tested according to GB 13917.1 ~ 13917.7.

5.4.2 Toxic powder, poison pen and repellent are tested according to GB/T

17322.9 ~ 17322.10.

5.4.3 Unlisted dosage form products are implemented according to the methods in relevant national product standards.

5.5 Thermal storage stability

5.5.1 Mosquito coil

Take one coil from the middle of one box of test samples to crush. Pass the

0.154mm (100 mesh/inch) standard sample sieve. Take half of it and seal it in a Teflon reagent bottle (the other half is tested for active ingredient content).

Then place it in a thermostat at (54±2)°C for 14d. After taking out the sample, test and calculate the degradation rate according to the method for determining the content of active ingredient within 24h.

5.5.2 Electrothermal mosquito tablet incense

The test sample shall be the electrothermal mosquito tablet incense in the same row as before storage. The test sample (with aluminum foil packaging) is placed in a (54±2)°C thermostatic chamber for 14d. After taking out the sample, test and calculate the degradation rate according to the method for determining the content of active ingredient within 24h.

5.5.3 Electrothermal mosquito liquid incense

Take a part of a bottle of test sample as the active ingredient content. Screw the outer cover of the rest part into the original packaging. Then place in a (54±2)°C thermostatic chamber for 14d. After taking out the sample, test and calculate the degradation rate according to the method for determining the content of active ingredient within 24h.

Liquid medicine is poured into a measuring cylinder or weighed with a balance.

Read out the test value (measuring cylinder division value. 0.1mL; balance division value. 0.1g).

5.9 Internal pressure of insecticide aerosol

5.9.1 Instruments

5.9.1.1 Pressure gauge. range is 0~1.6MPa, accuracy is level 2.5.

5.9.1.2 Special joint.

5.9.1.3 Timer.

5.9.1.4 Constant temperature water bath. temperature control accuracy is ±2°C.

5.9.2 Test steps

Correctly press the valve actuator according to product description requirements. Eliminate the air trapped in valves and straws. Then place the sample in a (55±2)°C water bath. Immerse the water to four-fifths of the height of the tank. Maintain it at the constant temperature for 30min. Wear thick leather gloves. Remove the sample and dry it quickly. Unplug the valve actuator. Align the pressure gauge inlet with the valve stem. Press hard. After the pressure gauge pointer stabilizes, write down the pressure gauge reading. The maximum value of three measurements shall prevail.

5.10 Net content of insecticide aerosol

5.10.1 Net volume of insecticide aerosol

5.10.1.1 Instruments

5.10.1.1.1 Glass aerosol test tube with scale. capacity is 90mL, minimum division value is 1mL.

5.10.1.1.2 Balance. division value is not less than 0.01g.

5.10.1.2 Test temperature

The test temperature is (25±3)°C.

5.10.1.3 Test steps

Take the sample and weigh its mass m3.Assemble the glass aerosol test tube.

Use a valve without a straw. Wipe the glass aerosol test tube clean. First inject a proper amount of propellant, about 10mL. Then spray empty and weigh its mass m4.

Annex A (normative)

Method for determining content of active ingredients in mosquito coils

A.1 Identification test

This identification test can be carried out simultaneously with the determination of the content of active ingredients. Under the same chromatographic operating conditions, the relative difference between the retention time of a chromatographic peak in the sample solution and the retention time of the active ingredient in the standard shall be within 1.5%.

A.2 Method summary

The sample uses dibutyl phthalate or dipentyl phthalate as the internal standard.

Conduct gas chromatography separation and determination on internal coated

SE-54 capillary column.

A.2.1 Instruments

A.2.1.1 Gas chromatograph. with hydrogen flame ionization detector.

A.2.1.2 Chromatography column. Phi0.25mm × 30m × 0.25µm, capillary column

coated with SE-54.

A.2.1.3 Micro syringe. 10µL.

A.2.1.4 Ground-mouth triangular flask.

A.2.1.5 Balance. division value is 0.1mg.

A.2.1.6 Grinder.

A.2.1.7 Sieve. standard sample sieve 0.154mm (100 mesh/inch).

A.2.1.8 Filter paper.

A.2.1.9 Oscillator.

A.2.2 Reagents

A.2.2.1 Internal standard substance. dibutyl phthalate or dipentyl phthalate, without interference impurities.

A.2.2.2 Solvents. acetone, methanol (analytical reagent).

Annex B (normative)

Method for determining content of active ingredients in electrothermal mosquito tablet incense

B.1 Identification test

This identification test can be carried out simultaneously with the determination of the content of active ingredients. Under the same chromatographic operating conditions, the relative difference between the retention time of a chromatographic peak in the sample solution and the retention time of the active ingredient in the standard solution shall be within 1.5%.

B.2 Method summary

The sample uses dibutyl phthalate or diisooctyl phthalate as the internal standard substance. Conduct gas chromatography separation and determination on internal coated SE-54 capillary column.

B.2.1 Instruments

B.2.1.1 Gas chromatograph. with hydrogen flame ionization detector.

B.2.1.2 Chromatography column. Phi0.25mm × 30m × 0.25µm, capillary column

coated with SE-54.

B.2.1.3 Micro syringe. 10µL.

B.2.1.4 Ground-mouth test tube.

B.2.1.5 Ground-mouth triangular flask.

B.2.1.6 Balance. division value is 0.1mg.

B.2.2 Reagents

B.2.2.1 Internal standard substance. dibutyl phthalate or diisooctyl phthalate, without interference impurities.

B.2.2.2 Solvents. acetone, methanol (analytical reagent).

B.2.2.3 Standard samples. allethrin, propargyl, etc.

B.2.3 Gas chromatography conditions

Annex C (normative)

Method for determining content of active ingredients in electrothermal mosquito liquid incense

C.1 Identification test

This identification test can be carried out simultaneously with the determination of the content of active ingredients. Under the same chromatographic operating conditions, the relative difference between the retention time of a chromatographic peak in the sample solution and the retention time of the active ingredient in the standard solution shall be within 1.5%.

C.2 Method summary

The sample uses dibutyl phthalate as the internal standard substance. Conduct gas chromatography separation and determination on internal coated SE-54 capillary column.

C.2.1 Instruments

C.2.1.1 Gas chromatograph. with hydrogen flame ionization detector.

C.2.1.2 Chromatography column. Phi0.25mm × 30m × 0.25µm, capillary column

coated with SE-54.

C.2.1.3 Micro syringe. 10µL.

C.2.1.4 Ground-mouth test tube.

C.2.1.5 Ground-mouth triangular flask.

C.2.1.6 Balance. division value is 0.1mg.

C.2.1.7 Dropper with rubber head.

C.2.2 Reagents

C.2.2.1 Internal standard substance. dibutyl phthalate, free of interfering

impurities.

C.2.2.2 Solvents. acetone, methanol (analytical reagent).

C.2.2.3 Standard samples. allethrin, propargyrin, etc.

C.2.3 Gas chromatography conditions

C.2.3.1 Temperature

C.2.3.1.1 Column temperature. 220°C.

C.2.3.1.2 Gasification temperature. 250°C.

C.2.3.1.3 Detector temperature. 250°C.

C.2.3.2 Carrier gas. nitrogen.

The above operating conditions are typical operating parameters. According to the characteristics of different instruments, the given operating conditions can be adjusted appropriately in order to obtain the best results.

C.3 Preparation of standard solution

In a ground-mouth test tube, accurately weigh 0.03g~0.04g (to the nearest of

0.0002g) of standard sample equivalent to the sample to be tested. Then weigh

0.015g~0.025g (to the nearest of 0.0002g) of dibutyl phthalate. Add methanol- acetone mixed solution. After fully dissolved, stopper and shake well, put in the refrigerator for use.

C.4 Preparation of sample solution

In a ground-mouth test tube, accurately weigh 1g~4g (to the nearest of 0.0002g, the ingredient to be tested is estimated about 0.03g~0.04g) of electrothermal mosquito liquid incense to be analyzed. Then weigh 0.015g~0.025g (to the nearest of 0.0002g) of dibutyl phthalate. Stopper and shake well, to be analyzed.

C.5 Determination

Under chromatographic conditions in C.2.3, after the instrument is stable, use a micro syringe to continuously inject standard sample solution until the peak area ratio of two adjacent needles and internal standard changes less than

1.5%. Conduct sample injection analysis in the order of standard sample solution, sample solution, sample solution, and standard sample solution.

C.6 Calculation

Respectively average the ratio of the peak area of the sample peak to the internal standard in the measured sample solution and the area ratio of the peak of the two internal standards to the peak of the standard sample. According to formula (C.1) and formula (C.2), calculate the mass fraction of the active ingredient to be measured, Mx.

Correction factor.

D.2.3 Gas chromatography conditions

D.2.3.1 Temperature. the initial temperature of the column temperature is 220°C, the retention time is 13min; the termination temperature is 260°C, the retention time is 20 min; the heating rate is 20°C/min.

Gasification temperature. 270°C.

Detector temperature. 270°C.

D.2.3.2 Carrier gas. nitrogen.

The above operating conditions are typical operating parameters. According to the characteristics of different instruments, the given operating conditions can be adjusted appropriately in order to obtain the best results.

D.3 Preparation of internal standard solution

In a 100mL volumetric flask, weigh 0.3g~0.5g (to the nearest of 0.0002g) of corresponding internal standard substance. Use acetone or absolute ethanol to dissolve and set volume to scale. Shake well for use.

D.4 Preparation of standard solution

In a 50mL volumetric flask, accurately weigh various standard samples of an amount equivalent to the sample to be tested, m1 (to the nearest of 0.0002g).

Add 5mL of internal standard solution. Set volume after complete dilution.

Stopper and shake well. Put in the refrigerator to use.

Method One.

D.5 Preparation of sample solution

In a clean 50mL volumetric flask, add 10mL of acetone or absolute ethanol.

Shake the entire bottle of aerosol. Pre-spray several times. Use a sprinkler with a catheter (the end of the catheter is immersed in acetone or absolute ethanol) and slowly spray about 10g of the drug solution (the mass m2 is obtained by the weight reduction method, to the nearest of 0.001g). It can be placed in a 55°C water bath. After slowly removing the propellant (until there are no obvious bubbles), after adding 5mL of internal standard solution, use acetone or absolute ethanol to set volume to the scale. Shake well for use.

D.6 Determination

Under chromatographic conditions in D.2.3, after the instrument is stable, use a micro syringe to continuously inject standard sample solution until the peak area ratio of two adjacent needles and internal standard changes less than

D.8 Preparation of standard solution

In a ground-mouth test tube, accurately weigh various standard samples of an amount equivalent to the sample to be tested (to the nearest of 0.0002g). Then weigh 0.015g~0.025g (to the nearest of 0.0002g) of dipentyl phthalate. Add 5mL of acetone solution. After complete dilution, stopper and shake well. Put in the refrigerator to use.

D.9 Sample pre-processing

Take a can of aerosol sample. Place it in a low temperature box at about -15°C for 4h and take it out. Open a small hole with a diameter of about 0.2mm at the top of the tank. Place in 46°C water bath for 1h. Let the propellant slowly evaporate. Enlarge the hole. Pour out the liquid.

D.10 Preparation of sample solution

In a ground-mouth test tube, accurately weigh 10g of aerosol feed (to the nearest of 0.0002g, depending on the amount of substance to be tested). Then weigh 0.015g~0.025g of dipentyl phthalate. Stopper and shake well, to be analyzed.

D.11 Determination

Under chromatographic conditions in D.2.3, after the instrument is stable, use a micro syringe to continuously inject standard sample solution until the peak area ratio of two adjacent needles and internal standard changes less than

1.5%. Conduct sample injection analysis in the order of standard sample solution, sample solution, sample solution, and standard sample solution.

D.12 Calculation

Respectively average the ratio of the peak area of the sample peak to the internal standard in the measured sample solution and the area ratio of the peak of the two internal standards to the peak of the standard sample. According to formula (D.3), formula (D.4) and formula (D.5), calculate the mass fraction of the component to be tested, Mx.

Correction factor.

Mass fraction of ingredient to be tested.

cstandard

......