Some standard content:
National Standard of the People's Republic of China
Gibberellins technical
Other names, structural formulas and basic physicochemical parameters of gibberellins are as follows: ISO common name: gibberellins
Trade name: Gibberellins crystalline powder, 920
CIPAC digital code: 307
Active ingredient: Gibberellic acid GA:
GB15955--1995
Chemical name: 2B4a, 7-trihydroxy-1-methyl-8-methylene-4aa, 46.2B-gibberellins-3-ene-1a, 10B-dicarboxylic acid-1.4a-lactone. Structural formula:
Empirical formula: C19H22Os
Relative molecular mass: 346.37 (according to the 1991 international relative atomic mass) Biological properties: plant growth regulator
Melting point: 223~225℃ (decomposition)
Solubility: 5g/L in water. Easily soluble in organic solvents such as alcohols, acetone, ethyl acetate, and also soluble in sodium bicarbonate and pH 6.2 phosphate buffer solution.
Stability: Stable in dry state, relatively stable in acidic solution, and easily decomposed by alkali. Subject content and scope of application
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation and storage of gibberellin technical. This standard applies to gibberellin technical composed of gibberellin and impurities generated in its production. Gibberellin technical should be free of foreign impurities. 2 Reference standards
GB/T613 General method for determination of specific rotation of chemical reagents GB/T1604 Acceptance rules for pesticides
GB/T1605 Sampling method for commercial pesticides
GB3796 General rules for pesticide packaging
3 Technical requirements
3.1 Appearance
White to slightly yellow crystalline powder.
Approved by the State Administration of Technical Supervision on December 21, 1995, and implemented on August 1, 1996
3.2 Gibberellic acid technical shall meet the requirements of the following table: Item
Gibberellic acid GA: Content, %
Loss on drying, %
Specific optical rotation [a]°
Test method
GB15955--1995
Superior product
First-class product
Qualified product
Unless otherwise specified, the reagents used in this test are all analytically pure reagents, and the water shall meet the requirements of the third-grade water in GB/T6682. 4.1 Appearance inspection
Visual observation method. bZxz.net
4.2 Determination of gibberellic acid GA: content
4.2.1 Identification test
4.2.1.1 Identification test 1
This identification test can be carried out simultaneously with the determination of gibberellic acid GA: content. 4.2.1.2 Identification test 2
Take a small amount of this product and dissolve it in 2mL concentrated sulfuric acid. A slightly red solution with green fluorescence should be formed. 4.2.2 High pressure liquid chromatography
4.2.2.1 Method summary
The sample is dissolved in methanol and separated by a C18 reverse phase liquid chromatography column. The ultraviolet detector is used for determination. The mobile phase is methanol + water + formic acid. The gibberellic acid GA: content is determined by the external standard method. 4.2.2.2 Reagents and solutions
Methanol (GB/T 683)
Formic acid (HG/T 1296);
Distilled water: twice redistilled;
erythrocytic acid GA, standard sample: known content of more than 98%. 4.2.2.3 Instruments
High performance liquid chromatograph: with adjustable wavelength UV detector, chromatographic column: length 150mm, inner diameter 4.6mm, internal ODS-C1g5μ); data processor:
Micro syringe: 50uL.
4.2.2.4 Chromatographic operating conditions
Column temperature: room temperature:
Detection wavelength: 210nm,
Mobile phase: methanol + water + formic acid = 40 + 60 + 0.05 (V/V); flow rate: 0.8 mL/min;
Injection volume: 20μL (quantitative tube injection); retention time: GA: about 7.8min,
Liquid chromatogram is shown in Figure 1.
(Analysts can make appropriate adjustments to the above-mentioned liquid chromatography operating conditions according to the characteristics of the instrument in order to obtain the best separation conditions).
4.2.2.5 Preparation of standard solution
GB15955-1995
Figure 1 Gibberellic acid GA: Liquid phase chromatogram
Figure 1 is gibberellic acid GA,
, 894
Weigh 0.08g (accurate to 0.0002g) of gibberellic acid GA3 standard sample in a 100mL volumetric flask, dilute to scale with methanol, and shake well. Accurately pipette 5mL of the solution into a 50mL volumetric flask, dilute to scale with mobile phase, shake well, and set aside. 4.2.2.6 Preparation of gibberellin technical sample
Weigh 0.1g (accurate to 0.0002g) of the sample into a 100mL volumetric flask, dilute to scale with methanol, and shake well. Accurately pipette 5mL of the solution into a 50mL volumetric flask, dilute to scale with mobile phase, shake well, and set aside. 4.2.2.7 Determination
Under the chromatographic conditions of 5, 2, 2, 4, after the instrument is stable, first inject several needles of standard solution until the difference between the peak areas of two adjacent needles is less than 1.5%, and then analyze in the following order: standard solution, sample solution, sample solution, standard solution. 4.2.2.8 Calculate the mass percentage of red acid GA: in the
sample X1, calculated according to formula (1): X, = Am:W
The average peak area of GA: in the same standard solution measured by two injections before and after, where: A,—
A2—the average peak area of GA: in the same sample solution measured by two injections before and after; m1——GA: the weight of the standard sample, g;
m2-the weight of the sample, g;
-GA: the percentage of the standard sample.
4.2.2.9 Allowable difference
The difference between the two determination results shall not exceed 1.5%. 4.3 Determination of loss on drying
4.3.1 Instruments and equipment
Flat weighing bottle: $40mm
Electrical constant temperature drying oven: ±2℃
4.3.2 Determination steps
(1)
Weigh about 18 grams of the mixed sample (accurate to 0.0002g) into a pre-weighed weighing bottle, put the bottle into a constant temperature oven at 105℃±2℃ to dry, take it out after 1 hour, cool it in a dryer for 1 hour and then weigh it. The loss on drying %(X,) is calculated according to formula (2):
Where: ma is the mass of the sample after drying, g; m is the mass of the sample, g.
4.4 Determination of specific rotation
GB 15955—1995
Perform according to GB/T613, where the concentration of ethanol solution is 0.1g/mL. If the sample is turbid after dissolution, it should be filtered with rapid quantitative filter paper before determination. The result is calculated according to formula (3): [α
(ααo)·V
ms(1 -- 0.01X,)l
Wherein: [αJ召——Specific optical rotation measured at 20℃ using the wavelength of the sodium spectrum D line; ar
5 Inspection rules
5.1 Sampling method
Optical rotation of the sample;
Optical rotation of the blank solution;
Dilution volume of the sample, mL,
Mass of the sample, g;
Loss on drying of the sample, %;
Length of the polarimeter tube, dm.
Sampling shall be carried out in accordance with GB/T1605. The packages to be sampled shall be determined by random method, and the final sampling volume shall generally not be less than 20g. 5.2 Acceptance rules
Acceptance shall be carried out in accordance with GB/T1604.
6 Marking, packaging, transportation and storage
6.1 The packaging and marking of the GA3 technical shall comply with the relevant provisions of GB3796 and shall be marked with a trademark. 6.2 The GA3 technical shall be packaged in small plastic bags. Each bag contains 1g. Each 100g is a box. Each 20 boxes is a carton. (3)
6.3 Other forms of packaging may be used according to user requirements or agreement between the supply and demand parties, but they must comply with the relevant provisions of GB3796. 6.4 Avoid impact and rain during transportation and keep away from fire. Be careful when handling and loading. 6.5 The packaged items shall be stored in a cool, dry place, fireproof and moisture-proof. They shall not be placed in the open air or stacked with toxic substances, flammable and explosive materials, or alkaline substances.
6.6 Warranty period: Under the specified storage conditions, the warranty period for the intact gibberellin technical is at least two years from the date of production. During the warranty period, the gibberellin content should meet the index requirements of this standard. Additional remarks:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is technically managed by the Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Shanghai Pesticide Research Institute. The main drafters of this standard are Ye Wenbing, Xu Fengbao, Guo Jiwen, Xue Liandi, Wu Xiang, and Huang Wenxiao.
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