GB 19337-2003 Avermectin emulsifiable concentrate

This standard specifies the requirements, test methods, marking, labeling, packaging and storage of avermectin emulsifiable concentrate. This standard applies to avermectin emulsifiable concentrate prepared by dissolving avermectin technical and emulsifier in a suitable solvent. GB 19337-2003 Abamectin emulsifiable concentrate GB19337-2003 standard download decompression password: www.bzxz.net

Chapter 3 and Chapter 5 of this standard are mandatory, and the rest are recommended. This standard was proposed by the former State Bureau of Petroleum and Chemical Industry. This standard is under the jurisdiction of the National Technical Committee for Standardization of Pesticides (SAC/TC133). The Secretariat of the National Technical Committee for Standardization of Pesticides is entrusted with the interpretation of this standard. The responsible drafting unit of this standard: Shenyang Chemical Research Institute. GB19337—2003
Participating drafting units of this standard: Zhejiang Haizheng Chemical Co., Ltd., Hebei Weiyuan Biochemical Co., Ltd., North China Pharmaceutical Group Ainuo Co., Ltd.
Main drafters of this standard: Mei Baogui, Li Xiujie, Lin Yuancheng, Lu Li, Liu Yingxin, Ci Suying. 1
Avermectin EC
Other names, structural formulas and basic physicochemical parameters of the active ingredient avermectin in this product are as follows: ISO common name: Abamectin
GB19337—2003
Chemical name: (10E,14E,16E,22Z)-(1R,4S,5'S,6S,6'S,8R,12S,13S,20R,21 R24S)-6'-[(S)-sec-butyl]-21,24-dihydroxy-5,11,13,22-tetramethyl-2-oxo-3,7,19-trioxatetracyclo[15.6.1.14,8020.24]pentacosyl-10,14,16,22-tetraene-6-spiro-2'-(5'6'-dihydro-2'H-pyran)-12-yl 2,6-dideoxy-4-O-(2,6-dideoxy- 3-O-methyl-α-1-(2-(2-nitro-1-nitro-2-yl)-3-O-methyl-α-L-arabinohexopyranos ... -Trioxatetracyclo[15.6.1.14.8O20,24]pentacrylic acid-10,14,16,22-tetraene-6-spiro-2'-(5',6'-dihydro-2'H-pyranose)-12-yl 2,6-dideoxy-4-0 (2,6-dideoxy-3-O-methyl-α-L-arabinopyranose)-3-O-methyl-α-L-arabinopyranose (II) (4:1) mixture.
Structural formula:
(1) R=CH(Abamectin Bia)
(2) R=CH,CH,(Abamectin Bi)
Empirical formula:(1) BibC4HO14,(2)Bi. CagHz2 O14H
Relative molecular mass: B1b, 858.1B1a, 872.1 (according to the 1995 international relative atomic mass) Biological activity: insecticide
Melting point: 150℃～155℃
Vapor pressure (20℃): <2×10-4mPa
Solubility (21℃, g/L): water (7～10)×10-6, toluene 350, acetone 100, isopropanol 70, chloroform 25, ethanol 20, methanol 19.5, n-butanol 10, cyclohexane 6
Stability: Good stability in aqueous solution with a pH value of 5~~9 (25℃); sensitive to strong acids and alkalis; under ultraviolet light, it will first convert into 8,9-Z isomers and then degrade into unknown products. Scope
This standard specifies the requirements, test methods, marking, labeling, packaging, storage and transportation of avermectin emulsifiable concentrates. This standard applies to avermectin emulsifiable concentrates prepared by dissolving avermectin technical and emulsifiers in suitable solvents. GB 19337-2003
2 Normative references
The clauses in the following documents become the clauses of this standard through reference in this standard. For all dated referenced documents, all subsequent amendments (excluding errata) or revisions are not applicable to this standard. However, the parties who reach an agreement based on this standard are encouraged to study whether the latest versions of these documents can be used. For all undated referenced documents, the latest versions shall apply to this standard. GB/T 1600
GB/T 1601
GB/T 1603
GB/T 1604
GB/T 1605
Method for determination of moisture content in pesticides
Method for determination of pH value in pesticides
Method for determination of stability of pesticide emulsions
Acceptance rules for commercial pesticides
Method for sampling commercial pesticides
GB4838 Packaging of pesticide emulsifiable concentrates
GB19336 Abamectin technical
3 Requirements
Appearance: It should be a stable homogeneous liquid without visible suspended matter and precipitation. 3.1
3.2 The technical used to prepare Abamectin emulsifiable concentrates shall comply with the requirements of GB19336. 3.3 Abamectin emulsifiable concentrates shall comply with the requirements of Table 1. Table 1 Control Items of Abamectin Emulsifiable Concentrate
Mass fraction of Abamectin (Bra+Bn)/%α(Bra/Bh)
Mass fraction of water/%
pH range
Emulsion stability (diluted 200 times)
"Low temperature stability"
Hot storage stability"
Low temperature and hot storage stability tests shall be tested at least once every 3 months under normal production conditions. 4 Test methods
4.1 Sampling
Indicated value (should be accurate to 0.1%)
Carry out in accordance with the "Sampling of Liquid Preparations" method in GB/T1605. The sampling packages shall be determined by the random number table method, and the final sampling volume shall be not less than 200 mL.
4.2 Identification test
High performance liquid chromatography This identification test can be carried out simultaneously with the determination of the content of Abamectin. Under the same chromatographic operating conditions, the relative differences between the retention times of two chromatographic peaks of the sample solution and the retention times of the avermectin Bi and B1 in the standard solution should be within 1.5%.
4.3 Determination of the mass fraction of avermectin (B1.+Bb) and α(B1a/B) 4.3.1 Summary of the method
The sample was dissolved in methanol, and methanol + acetonitrile + water was used as the mobile phase. A stainless steel column with Nova-PakCls as the filler and an ultraviolet detector (245 nm) were used to separate the avermectin in the sample by reverse phase high performance liquid chromatography, and the external standard method was used for quantification. 4.3.2 Reagents and solutions
Methanol: chromatographic grade;
Water: freshly distilled water;
B: chromatographic grade;
Avermectin standard: the mass fraction of known avermectin (Bl.+Bib) is ≥98.0%. 4.3.3 Instruments
High performance liquid chromatograph: with variable wavelength ultraviolet detector; chromatography data processor;
GB 19337-2003
Chromatographic column: 150mmX3.9mm (id) stainless steel column, filled with Nova-PakC18, 5μm filler (or chromatographic column with equivalent effect);
Filter: pore size of filter membrane is about 0.45μm;
Micro-injector: 50μL;
Quantitative injection tube: 5uL;
Ultrasonic cleaner.
4.3.4 HPLC operating conditions
Mobile phase: (methanol: acetonitrile: water) -38:38:24, filtered through a filter membrane and degassed; flow rate: 1.0 mL/min;
Column temperature: room temperature (temperature difference should not exceed 2°C), detection wavelength: 245nm;
Injection volume: 5μL;
Retention time: Bla 15.6 min, Bib 11.3 min. The above operating parameters are typical, and the given operating parameters can be appropriately adjusted according to the characteristics of different instruments in order to obtain the best effect. A typical avermectin emulsifiable concentrate HPLC chromatogram is shown in Figure 1. 1
-avermectin Bi. ;
-avermectin Bib.
Figure 1 High performance liquid chromatogram of avermectin emulsifiable concentrate 4.3.5 Determination steps
4.3.5.1 Preparation of standard solution
Weigh 0.05g of avermectin standard sample (accurate to 0.0002g), place it in a 100mL volumetric flask, dissolve it in methanol and dilute it to the scale, and shake it well.
GB 19337—2003
4.3.5.2 Preparation of sample solution
Weigh 0.05g of sample containing avermectin (accurate to 0.0002g), placed in a 100mL volumetric flask, dissolved in methanol and diluted to the scale, shake well.
4.3.5.3 Determination
Under the above operating conditions, after the instrument is stable, inject several injections of standard solution continuously until the relative change of the peak area of ​​avermectin (Bia+Bib) between two adjacent injections is less than 1.5%, and then perform determination in the order of standard solution, sample solution, sample solution, and standard solution. 4.3.6 Calculation The mass fraction w (%) of avermectin (Bi.+Bl) in the sample shall be calculated according to formula (1): e
Wherein:
Az Xm, Xp
Ai--the average value of the sum of the peak areas of avermectin Bila and Brb in the standard solution; A2--the average value of the sum of the peak areas of avermectin Bia and Bib in the sample solution; ml--the mass of the standard sample, in grams (g); m2
the mass of the sample, in grams (g);
--the mass fraction of avermectin (B1a+Bib) in the standard sample, %. p--|tt||α(Bia/Bib) in the sample shall be calculated according to formula (2): α(Bia/Bib) =
Wherein:
In the two sample solutions, avermectin Bi. The average value of the sum of the peak areas; - The average value of the sum of the peak areas of avermectin Bb in the two sample solutions. 4.3.7 Permissible difference
- (2)
The relative difference between the results of two parallel determinations of a sample with a mass fraction of avermectin greater than 1.0% shall not be greater than 5%; the relative difference between the results of two parallel determinations of a sample with a mass fraction of avermectin less than 1.0% shall not be greater than 10%. Take the arithmetic mean as the determination result.
4.4 Determination of moisture
Carry out in accordance with the "Karl Fischer method" in GB/T1600. It is allowed to use a micro-moisture meter with equivalent accuracy. 4.5 Determination of pH value
Carry out in accordance with GB/T 1601.
4.6 Emulsion stability test
Carry out in accordance with GB/T1603; no floating oil on the top, no sinking oil and no precipitation on the bottom are qualified. 4.7 Low temperature stability test
4.7.1 Method summary
The sample is kept at 0℃ for 1 hour, and the presence of solid and oily matter is recorded. It is then stored at 0℃ for 7 days. The solid precipitate is centrifuged to settle, and its volume is recorded.
4.7.2 Apparatus
Refrigerator: maintained at 0℃±2℃;
Centrifuge tube: 100mL, with scale on the bottom of the tube accurate to 0.05mL; Centrifuge: Matched with centrifuge tube.
4.7.3 Test steps
Take 100mL±1.0mL of the sample and add it to the centrifuge tube, cool it to 0℃±2℃ in the refrigerator, and keep the centrifuge tube and its contents at 0℃±2℃ for 1 hour. Stir once every 15min for 15s each time, and check and record the presence of solid or oily matter. Put 4
GB 193372003
centrifuge tubes back into the refrigerator and continue to place them at 0℃±2℃ for 7 days. Take out the centrifuge tubes, place them at room temperature (not exceeding 20℃) for 3 hours, and centrifuge for 15 minutes (the relative centrifugal force at the top of the tube is 500g~600g, g is the acceleration of gravity). Record the volume of the precipitate at the bottom of the tube (accurate to 0.05mL). The precipitate is qualified if it does not exceed 0.3mL. 4.8 Thermal storage stability test
4.8.1 Instruments
Thermostatic box (or constant temperature water bath): 54℃±2℃; bottle (or glass bottle with stopper that can still be sealed at 54℃): 50mL; medical syringe, 50mL.
4.8.2 Determination steps
Use a syringe to inject about 30mL of the sample into a clean bottle (or glass bottle) (avoid the sample from contacting the bottleneck), place the bottle in an ice-salt bath to cool, and quickly seal it with a high-temperature flame (avoid solvent volatilization). Seal at least 3 bottles and weigh them separately. Place the sealed bottle in a metal container, and then place the metal container in a 54℃±2℃ constant temperature box (or water bath) for 14 days, take it out and cool it to room temperature, wipe the outside of the bottle and weigh it separately. For samples that have not changed in mass, test the avermectin content and emulsion stability within 24 hours. The mass fraction of avermectin should not be less than 95% of the mass fraction before storage, and the emulsion stability should meet the requirements of this standard. 4.9 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method shall be used for the processing of limit values. 5.1 The marking, labeling and packaging of Abamectin EC shall comply with the provisions of GB4838. 5.2 Abamectin EC shall be packaged in brown glass bottles, aluminum bottles or fluoride bottles with inner plugs and outer caps, with a net content of 50g (mL), 100g (mL), 250g (mL), 500g (mL); the outer packaging shall be calcium plastic boxes or corrugated paper boxes, and the net content of each box shall not exceed 15kg. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the provisions of GB4838. 5.4 The packages shall be stored in a ventilated and dry warehouse. 5.5 During storage and transportation, strictly prevent moisture and sunlight, do not mix with food, seeds, feed, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Abamectin EC is of low toxicity. Abamectin agents should be avoided from contaminating water sources. Avoid contact of the agent with the skin to prevent poisoning due to absorption through the skin. Avoid splashing the agent into the eyes or inhaling the drug mist. If the agent contacts the skin or clothing, rinse immediately with plenty of water and soap; if it splashes into the eyes, rinse with plenty of water and consult a doctor; if it is taken by mistake, induce vomiting immediately and give the patient ipecac syrup or ephedrine, but never feed anything or induce vomiting to a comatose patient. Avoid using drugs that can enhance the activity of -aminobutyric acid (such as barbiturates, etc.). 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of avermectin emulsifiable concentrate is 2 years from the date of production. During the warranty period, the mass fraction of water is allowed to rise to 1.0%, and all other indicators shall meet the requirements of this standard.Add 0mL of sample to a centrifuge tube, cool it to 0℃±2℃ in a refrigerator, keep the centrifuge tube and its contents at 0℃±2℃ for 1h, stir it once every 15min, 15s each time, check and record whether there is solid or oily precipitation. Put the 4
GB 193372003
centrifuge tube back into the refrigerator, keep it at 0℃±2℃ for 7d, take out the centrifuge tube, let it stand at room temperature (not exceeding 20℃) for 3h, and centrifuge for 15min (the relative centrifugal force at the top of the tube is 500g~600g, g is the acceleration of gravity). Record the volume of the precipitate at the bottom of the tube (accurate to 0.05mL). The precipitate is qualified if it does not exceed 0.3mL. 4.8 Hot Storage Stability Test
4.8.1 Apparatus
Thermostatic box (or thermostatic water bath): 54℃±2℃; bottle (or glass bottle with stopper that can still be sealed at 54℃): 50mL; medical syringe, 50mL.
4.8.2 Determination steps
Use a syringe to inject about 30mL of sample into a clean bottle (or glass bottle) (avoid the sample from contacting the bottleneck), place the bottle in an ice-salt bath to cool, and quickly seal it with a high-temperature flame (avoid solvent volatilization). Seal at least 3 bottles and weigh them separately. Place the sealed bottle in a metal container, and then place the metal container in a thermostatic box (or water bath) at 54℃±2℃ for 14 days, take it out and cool it to room temperature, wipe the outside of the bottle and weigh it separately. For samples with no change in mass, test the avermectin content and emulsion stability within 24 hours. The mass fraction of avermectin should not be less than 95% of the mass fraction before storage, and the emulsion stability should meet the requirements of this standard. 4.9 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method shall be used for the processing of limit values. 5 Marking, labeling, packaging and storage and transportation
5.1 The marking, labeling and packaging of avermectin emulsifiable concentrate shall comply with the provisions of GB4838. 5.2 Abamectin emulsifiable concentrate shall be packaged in brown glass bottles, aluminum bottles or fluorinated bottles with inner plugs and outer caps, with a net content of 50g (mL), 100g (mL), 250g (mL), 500g (mL); the outer packaging shall be calcium plastic boxes or corrugated paper boxes, and the net content of each box shall not exceed 15kg. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the provisions of GB4838. 5.4 The packages should be stored in a ventilated and dry warehouse. 5.5 During storage and transportation, strictly prevent moisture and sunlight, do not mix with food, seeds, feed, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Abamectin EC is of low toxicity. Avoid contamination of water sources by Abamectin agents. Avoid contact of agents with skin to avoid poisoning through skin absorption. Avoid splashing agents into eyes or inhaling drug mist. If the agent contacts skin or clothes, rinse immediately with plenty of water and soap; if splashed into eyes, rinse with plenty of water and seek medical treatment; if taken by mistake, induce vomiting immediately and give the patient ipecac syrup or ephedrine, but do not feed anything or induce vomiting to patients who are already unconscious. Avoid using drugs that can enhance the activity of -aminobutyric acid (such as barbiturates, etc.). 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of Abamectin EC is 2 years from the date of production. During the warranty period, the mass fraction of water is allowed to rise to 1.0%, and all other indicators should meet the requirements of this standard.Add 0mL of sample to a centrifuge tube, cool it to 0℃±2℃ in a refrigerator, keep the centrifuge tube and its contents at 0℃±2℃ for 1h, stir it once every 15min, 15s each time, check and record whether there is solid or oily precipitation. Put the 4
GB 193372003
centrifuge tube back into the refrigerator, keep it at 0℃±2℃ for 7d, take out the centrifuge tube, let it stand at room temperature (not exceeding 20℃) for 3h, and centrifuge for 15min (the relative centrifugal force at the top of the tube is 500g~600g, g is the acceleration of gravity). Record the volume of the precipitate at the bottom of the tube (accurate to 0.05mL). The precipitate is qualified if it does not exceed 0.3mL. 4.8 Hot Storage Stability TestwwW.bzxz.Net
4.8.1 Apparatus
Thermostatic box (or thermostatic water bath): 54℃±2℃; bottle (or glass bottle with stopper that can still be sealed at 54℃): 50mL; medical syringe, 50mL.
4.8.2 Determination steps
Use a syringe to inject about 30mL of sample into a clean bottle (or glass bottle) (avoid the sample from contacting the bottleneck), place the bottle in an ice-salt bath to cool, and quickly seal it with a high-temperature flame (avoid solvent volatilization). Seal at least 3 bottles and weigh them separately. Place the sealed bottle in a metal container, and then place the metal container in a thermostatic box (or water bath) at 54℃±2℃ for 14 days, take it out and cool it to room temperature, wipe the outside of the bottle and weigh it separately. For samples with no change in mass, test the avermectin content and emulsion stability within 24 hours. The mass fraction of avermectin should not be less than 95% of the mass fraction before storage, and the emulsion stability should meet the requirements of this standard. 4.9 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method shall be used for the processing of limit values. 5 Marking, labeling, packaging and storage and transportation
5.1 The marking, labeling and packaging of avermectin emulsifiable concentrate shall comply with the provisions of GB4838. 5.2 Abamectin emulsifiable concentrate shall be packaged in brown glass bottles, aluminum bottles or fluorinated bottles with inner plugs and outer caps, with a net content of 50g (mL), 100g (mL), 250g (mL), 500g (mL); the outer packaging shall be calcium plastic boxes or corrugated paper boxes, and the net content of each box shall not exceed 15kg. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the provisions of GB4838. 5.4 The packages should be stored in a ventilated and dry warehouse. 5.5 During storage and transportation, strictly prevent moisture and sunlight, do not mix with food, seeds, feed, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Abamectin EC is of low toxicity. Avoid contamination of water sources by Abamectin agents. Avoid contact of agents with skin to avoid poisoning through skin absorption. Avoid splashing agents into eyes or inhaling drug mist. If the agent contacts skin or clothes, rinse immediately with plenty of water and soap; if splashed into eyes, rinse with plenty of water and seek medical treatment; if taken by mistake, induce vomiting immediately and give the patient ipecac syrup or ephedrine, but do not feed anything or induce vomiting to patients who are already unconscious. Avoid using drugs that can enhance the activity of -aminobutyric acid (such as barbiturates, etc.). 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of Abamectin EC is 2 years from the date of production. During the warranty period, the mass fraction of water is allowed to rise to 1.0%, and all other indicators should meet the requirements of this standard.
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