Some standard content:
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). This standard is entrusted to the Secretariat of the National Technical Committee for Standardization of Pesticides for interpretation. The responsible drafting unit of this standard: Shenyang Chemical Research Institute. GB19336-2003
Participating drafting units of this standard: Hebei Weiyuan Biochemical Co., Ltd., Zhejiang Haizheng Chemical Co., Ltd., North China Pharmaceutical Group Ainuo Co., Ltd.
Main drafters of this standard: Mei Baogui, Li Xiujie, Lu Li, Lin Yuancheng, Liu Yingxin, Ci Suying. I
Avermectin technical
Other names, structural formulas and basic physicochemical parameters of the active ingredient avermectin of this product are as follows: ISO common name: Abamectin
GB19336--2003
Chemical name: (10E,14E,16E,22Z)-(1R,4S,5'S,6S,6'S,8R,12S,13S,20R,21R,24 S)-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-L-arabinopyranosyl)-3-0-methyl-α-L-arabinopyranosyl (I) and (10E,14E,16E,22Z)-(1R,4S,5'S,6S,6'R,8R,12S,13S,20R,21R,24S)-21,22-dihydroxy-6-isopropyl-5',11,13,22-tetramethyl-2-oxo-3,7,19-trioxatetracyclo[15.6.1 .14,8020.24］Twenty-five-10,14,16,22-tetraene-6-spiro-2'-(5°,6°,-dihydro-2'H-pyranose)-12-yl 2,6-dideoxy-4-0(2,6-dideoxy-3-0-methyl-α-I-arabino-hexopyranose)-3-O-methyl-α-L-arabino-hexopyranose (II) (a mixture of 4:1.
Structural formula:
(1) R=CH,(Abamectin Bia)
(2) R-CH2CH:(Abamectin Bib)
Empirical formula: (1) BnC47HzO14, (2) Bi.C4gHz2O14H
Relative molecular mass: Bib, 858.1; Bla, 872.1 (according to the 1999 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-, Toluene 350 Acetone 10 0, isopropanol 70, chloroform 25, ethanol 20, methanol 19.5, n-butanol 10, cyclohexane 6
Stability: Good stability in aqueous solution (25℃) with pH value of 5-9; sensitive to strong acid and alkali; first converted to 8,9-z isomer under ultraviolet light, and then degraded into unknown products. 1 Scope
This standard specifies the requirements, test methods, marking, labeling, packaging and storage and transportation of avermectin technical. This standard applies to avermectin technical composed of avermectin and impurities generated in its production. 1
GB 19336--2003
2 Normative references
The clauses in the following documents become the clauses of this standard through reference in this standard. For all dated references, all subsequent amendments (excluding errata) or revisions are not applicable to this standard. However, parties to an agreement based on this standard are encouraged to study whether the latest versions of these documents can be used. For any undated referenced document, the latest version shall apply to this standard. GB/T1601 Determination of pH value of pesticides
GB/T 1604
Acceptance rules for commercial pesticides
GB/T1605 Sampling methods for commercial pesticides
GB3796 General rules for pesticide packaging
3 Requirements
3.1 Appearance: White to light yellow crystalline powder, without visible foreign impurities. 3.2 Avermectin technical shall meet the requirements of Table 1. Table 1
Mass fraction of avermectin (Bl.+Brb)/%
α(Bra/Bb)
Loss on drying/%
pH range"
Mass fraction of acetone insoluble matter/%
Control index of avermectin technical
Under normal production conditions, pH value and mass fraction of acetone insoluble matter shall be inspected at least once every 3 months. 4 Test method
4.1 Sampling
Carry out according to the "sampling of commercial technical drugs" method in GB/T1605. The sampling packages are determined by the random number table method; the final sampling volume shall not be less than 100g.
4.2 Identification test
High performance liquid chromatography-this identification test can be carried out simultaneously with the determination of avermectin content. Under the same chromatographic operating conditions, the retention time of two chromatographic peaks of the sample solution is the same as that of avermectin Bib and B1 in the standard solution. The relative difference of the retention time of the chromatographic peaks should be within 1.5%.
Infrared spectroscopy——
-There should be no obvious difference between the infrared absorption spectra of the sample and the standard sample in the range of 4000cm-1~400cm-1 (see Figure 1).
Figure 1 Infrared spectrum of avermectin standard sample
4. 3 Determination of mass fraction of avermectin (Br+Bb) and α(Ba/Bb) 4.3.1 Summary of the method
GB19336—2003
The sample was dissolved in methanol, and methanol+acetonitrile+water was used as the mobile phase. A stainless steel column with Nova-Pak C1s 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 quantified by the external standard method. 4.3.2 Reagents and solutions
Methanol: Chromatographic grade;
Water: Freshly distilled water;
Acetonitrile: Chromatographic grade;
Avermectin standard: Known Avermectin (Bla+B1) mass fraction ≥ 98.0%. 4.3.3 Instruments
High performance liquid chromatograph: with variable wavelength UV detector; Chromatographic data processor,
Chromatographic column: 150mm×3.9mm (id) stainless steel column, filled with Nova-PakCis, 5μm filler (or chromatographic column with equivalent effect);
Filter: pore size of filter membrane is about 0.45μm;
Micro-injector: 50μL;
Quantitative injection tube: 5μL,
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: Bia15.6min, Bib11.3min. The above operating parameters are typical. According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to obtain the best effect. The typical avermectin technical HPLC chromatogram is shown in Figure 2. 3
GB19336-2003
Avermectin Bla
Avermectin Bth.
4.3.5 Determination steps
4.3.5.1 Preparation of standard solution
Figure 2 High performance liquid chromatogram of avermectin original drug Weigh 0.05g of avermectin standard sample (accurate to 0.0002g), place it in a 100mL volumetric flask, dissolve it with methanol and dilute it to the scale, and shake it well.
4.3.5.2 Preparation of sample solution
Weigh 0.05g of sample containing avermectin (accurate to 0.0002g), place it in a 100mL volumetric flask, dissolve it with methanol and dilute it to the scale, and shake it well.
4.3.5.3 Determination
Under the above operating conditions, after the instrument is stable, continuously inject several needles of standard solution until the relative change of the peak area of two adjacent needles of avermectin (B1.+Blb) is less than 1.5%, then the determination is carried out in the order of standard solution, sample solution, sample solution and standard solution. 4.3.6 Calculation of the mass fraction wi (%) of avermectin (Bia+B) in the sample is calculated according to formula (1): i
Wherein:
A, Xmi Xp
A1—the average value of the sum of the peak areas of avermectins Bi and Bb in the standard solution; -the average value of the sum of the peak areas of avermectins B1 and B1, in the sample solution; A2
-the mass of the standard sample, in grams (g);
the mass of the standard sample, in grams (g);
the mass fraction of avermectin (B1a+Bib) in the standard sample, %. α(Bia/Bb) in the sample is calculated according to formula (2): α(Bra/Brb)—
Wherein:
in the two sample solutions, avermectin Bl. 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. (1)
·(2)
4.3.7 Allowable difference
GB 19336—2003
The difference between the two parallel determination results of avermectin mass fraction shall not be greater than 1.5%. The arithmetic mean value shall be taken as the determination result. 4.4 Determination of loss on drying
4.4.1 Instrument
Oven: 105℃±2℃;
Weighing bottle: inner diameter 70mm, height 40mm;
Dryer.
4.4.2 Determination steps
Put the weighing bottle in the oven for 1h, take it out and place it in the dryer to cool to room temperature, and weigh it (accurate to 0.0002g). Repeat the above steps until the weighing bottle reaches a constant weight. Place 2g of sample in the bottle, flatten it, weigh it (accurate to 0.01g), put the weighing bottle into the oven without covering it, dry it for 1h, take it out and put it into the desiccator to cool it to room temperature, weigh it (accurate to 0.0002g). 4.4.3 Calculate the drying loss X (%) in the sample according to formula (3): X = m = m2 × 100
Where:
mi——the mass of the sample and the weighing bottle before drying, in grams (g); m2——the mass of the sample and the weighing bottle after drying, in grams (g); m——the mass of the sample, in grams (g). 4.4.4 Allowable difference
The relative deviation of the results of two parallel determinations shall not exceed ±15%, and the arithmetic mean shall be taken as the determination result. 4.5 Determination of pH value
Determine according to GB/T1601. wwW.bzxz.Net
4.6 Determination of the mass fraction of acetone insoluble matter 4.6.1 Reagents and instruments
Acetone;
Erlenmeyer flask: 250mL, with matching condenser; Glass crucible: G3;
Oven: 105℃±2℃;
Suction filter flask: 500mL.
4.6.2 Determination method
· (3)
Weigh 10g of the sample (accurate to 0.01g), put it into an Erlenmeyer flask, add 100mL of acetone, heat and reflux for 15min, immediately filter through a filter that has reached a constant weight (accurate to 0.0002g), then wash the Erlenmeyer flask with 60mL of acetone three times, and filter it by suction. Dry it in an oven for 30min, take it out and cool it in a desiccator, and weigh it (accurate to 0.0002g). The mass fraction wz (%) of acetone insoluble matter in the sample is calculated according to formula (4): ml-mo×100
Wherein:
ml—total mass of acetone insoluble matter after drying, in grams (g); mo—mass of the crucible after constant weight, in grams (g); m—mass of the sample, in grams (g). 4.7 Inspection and acceptance of products
shall comply with the provisions of GB/T1604. For the processing of limit values, the rounded value comparison method shall be adopted. ·(4)
GB19336--2003
5 Marking, labeling, packaging and storage and transportation
5.1 The marking, labeling and packaging of avermectin technical shall comply with the provisions of GB3796. 5.2 Abamectin technical shall be packaged in clean, dry steel drums or cardboard drums lined with plastic bags, and the net content of each drum shall not exceed 25kg. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the provisions of GB3796. 5.4 The original drug packaging of avermectin 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, and feed, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Avermectin has high acute oral toxicity to mammals and is highly toxic. Avermectin agents should be avoided from contaminating water sources. Avoid contact of agents with the skin to avoid poisoning through skin absorption. Avoid splashing the agent into the eyes or inhaling the drug mist. If the agent contacts the skin or clothes, rinse it immediately with plenty of water and soap. If it splashes into the eyes, rinse it with plenty of water and ask a doctor for treatment; if it is 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 Acceptance period: The acceptance period for Avermectin technical is 1 month. From the date of delivery, the product quality acceptance shall be completed within 1 month, and all indicators shall meet the requirements of this standard.0002g). The mass fraction of acetone insoluble matter in the sample, wz (%), is calculated according to formula (4): ml-mo×100
Wherein:
ml—total mass of acetone insoluble matter after drying, in grams (g); mo—mass of the crucible after constant weight, in grams (g); m—mass of the sample, in grams (g). 4.7 Inspection and acceptance of products
shall comply with the provisions of GB/T1604. For the processing of limit values, the rounded value comparison method shall be adopted. ·(4)
GB19336--2003
5 Marking, labeling, packaging and storage and transportation
5.1 The marking, labeling and packaging of avermectin technical shall comply with the provisions of GB3796. 5.2 Abamectin technical shall be packaged in clean, dry steel drums or cardboard drums lined with plastic bags, and the net content of each drum shall not exceed 25kg. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the provisions of GB3796. 5.4 The original drug packaging of avermectin 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, and feed, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Avermectin has high acute oral toxicity to mammals and is highly toxic. Avermectin agents should be avoided from contaminating water sources. Avoid contact of agents with the skin to avoid poisoning through skin absorption. Avoid splashing the agent into the eyes or inhaling the drug mist. If the agent contacts the skin or clothes, rinse it immediately with plenty of water and soap. If it splashes into the eyes, rinse it with plenty of water and ask a doctor for treatment; if it is 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 Acceptance period: The acceptance period for Avermectin technical is 1 month. From the date of delivery, the product quality acceptance shall be completed within 1 month, and all indicators shall meet the requirements of this standard.0002g). The mass fraction of acetone insoluble matter in the sample, wz (%), is calculated according to formula (4): ml-mo×100
Wherein:
ml—total mass of acetone insoluble matter after drying, in grams (g); mo—mass of the crucible after constant weight, in grams (g); m—mass of the sample, in grams (g). 4.7 Inspection and acceptance of products
shall comply with the provisions of GB/T1604. For the processing of limit values, the rounded value comparison method shall be adopted. ·(4)
GB19336--2003
5 Marking, labeling, packaging and storage and transportation
5.1 The marking, labeling and packaging of avermectin technical shall comply with the provisions of GB3796. 5.2 Abamectin technical shall be packaged in clean, dry steel drums or cardboard drums lined with plastic bags, and the net content of each drum shall not exceed 25kg. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the provisions of GB3796. 5.4 The original drug packaging of avermectin 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, and feed, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Avermectin has high acute oral toxicity to mammals and is highly toxic. Avermectin agents should be avoided from contaminating water sources. Avoid contact of agents with the skin to avoid poisoning through skin absorption. Avoid splashing the agent into the eyes or inhaling the drug mist. If the agent contacts the skin or clothes, rinse it immediately with plenty of water and soap. If it splashes into the eyes, rinse it with plenty of water and ask a doctor for treatment; if it is 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 Acceptance period: The acceptance period for Avermectin technical is 1 month. From the date of delivery, the product quality acceptance shall be completed within 1 month, and all indicators shall meet the requirements of this standard.
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