GB 15955-2011Gibberellic acid technical material (English PDF)

3.1 Composition and appearance

This product should gibberellic acid and impurities generated in the production of the composition, it should be white to light yellow crystalline powder, free from visible foreign matter and filling Modifier.

3.2 Project and indicators

Gibberellic acid original drug should be consistent with the requirements in Table 1.

Table 1 gibberellic acid original drug control project indicators

Item Index

Gibberellic acid mass fraction /% >= 90.0 Loss on drying /% <= 0.5 the specific rotation ability alpham (20 °C, D)/[(°) · m2/kg] >= 80 Test Method 4

4.1 Sampling

According to GB/T 1605-2001 "on the original drug product sampling" approach. Random sampling method is determined by the package, the final amount of sample lot at 100g.

4.2 Identification Test

The identification test can be carried out simultaneously with the determination of the mass fraction of gibberellic acid. Under the same chromatographic operating conditions, the main sample solution chromatogram Retention time and peak standard solution of gibberellic acid chromatographic peak retention time, the relative difference should be less than 1.5%.

4.3 Determination of the mass fraction of gibberellic acid

4.3.1 Method summary

Sample dissolved in mobile phase, methanol - phosphoric acid as the mobile phase, use as filler to C18 stainless steel column and UV detector, for Gibberellic acid in the sample by reverse phase HPLC separation and determination of external standard.

4.3.2 Reagents and solutions

Phosphoric acid. AR;

Methanol. HPLC grade;

Water. The new secondary steam distilled water;

Phosphoric acid. [Psi] (water. phosphoric acid) = 2000.1;

Gibberellic acid standard sample. a known mass fraction w>=98.0%.

4.3.3 Instruments

High performance liquid chromatography. a variable wavelength UV detector and quantitative injection valve;

Chromatographic data processor or chromatography workstation;

Column. 250mm × 4.6mm (id) stainless steel column, built ZORBAX80ÅEXTENDC18 filler (or equivalent Other column effect);

Micro injector. 100µL;

Filter. pore size of about 0.45µm;

Ultrasonic cleaner.

4.3.4 HPLC operating conditions

Mobile phase. [Psi] (methanol. aqueous phosphoric acid solution) = 35.65;

Flow rate. 1.0mL/min;

Column temperature. room temperature (temperature change should not exceed 2 °C);

Detection wavelength. 210nm;

Injection volume. 10µL.

Retention time. gibberellic acid about 8.2min.

HPLC operating conditions described above, the Department of typical operating parameters, according to the characteristics of different instruments, given operating parameters to make appropriate adjustments to to obtain the best results. Typical gibberellic acid original drug HPLC is shown in Figure 1.

1 --- gibberellic acid.

Figure 1 HPLC gibberellic acid original drug

4.3.5 Measuring step

4.3.5.1 Preparation of standard solution

Weigh gibberellic acid standard about 0.05g (accurate to 0.0002g), placed in 100mL flask, add 35mL of methanol to dissolve, then Phosphoric acid aqueous solution was diluted to the mark.

4.3.5.2 Preparation of the sample solution

Weigh a sample containing about 0.05g of gibberellic acid (accurate to 0.0002g), placed in 100mL flask, add 35mL of methanol to dissolve, Phosphoric acid aqueous solution and then diluted to the mark. Filtered through a 0.45µm pore size filters.

4.3.5.3 Determination

Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles gibberellic acid peak area relative change After less than 1.5%, according to the solution, sample solution, sample solution, standard order of standard solution was measured.

4.3.6 Calculation

The two needle sample solution and measured before and after the two doses of the standard sample solution of gibberellic acid peak area were averaged. Sample gibberellic acid the mass fraction according to equation (1).

w1 = A2

· M1 · w

A1 · m2

Where.

w1 --- sample gibberellic acid content, expressed as a percentage;

A2 --- sample solution, gibberellic acid, the average peak area;

m1 --- gibberellic acid standard mass values in grams (g);

Mass fraction w --- standard samples gibberellic acid, expressed in%;

A1 --- standard solution, gibberellic acid, the average peak area;

Numerical m2 --- sample mass, in grams (g).

4.3.7 Allowable difference

The difference between two parallel determination results shall not be greater than 1.5%, the arithmetic mean value as a measurement result.

4.4 Determination of loss on drying

4.4.1 Instruments and Appliances

Oven. 105 °C ± 2 °C;

Weighing bottle. diameter 50mm, height 20mm;

Dryer.

4.4.2 Measuring step

The weighing bottle placed in 105 °C ± 2 °C oven baking 1h, and then into the dryer to cool to room temperature, weighed (accurate to 0.0002g).

Repeat the above steps until constant weight weighing bottle. In weighing bottle was weighed into a 1g sample (paved weighed accurate to 0.0002g). Will be referred Flask placed in an oven, bake uncovered 1h, the lid is removed and placed in the dryer to cool to room temperature, weighed (accurate to 0.0002g).

4.4.3 Calculation

Loss on drying of the sample according to equation (2).

w2 = m1-m2m

Where.

w2 --- Loss on drying, in%;

Mass m1 --- weighing bottle and sample before drying, in grams (g);

Mass m2 --- weighing bottle and sample after drying, in grams (g);

M --- the quality of the sample, in grams (g).

4.5 Determination of specific rotation ability

Performed according to GB/T 613-2007 requirements. Wherein the solution to be tested is gibberellic acid ethanol solution of the original drug at a concentration of 0.1g/mL. As solution After the sample is turbid solution was found, after application of rapid quantitative determination of filter paper. Sample specific rotation ability alpham (20 °C, D) [(°) · m2/kg], According to equation (3) Calculated.

alpham (20 °C, D) = 100

· Alpha · V

m 1-0.01w () 2 l

Where.

alpha --- measured rotation angle in degrees (°);

The V --- volume of the sample dilution in milliliters (mL of);

M --- the quality of the sample, in grams (g);

W2 --- Loss on drying of the sample, expressed in%;

--- optical tube length L, the unit decimeter (dm).

4.6 Product testing and acceptance

Shall comply with GB/T 1604's. Treatment of extreme values, using the rounding value comparison method.

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

5.1 Mark, label

Gibberellic acid original drug marking, labeling and packaging should comply with the provisions of GB 3796.

5.2 Packaging

Gibberellic acid original drug is appropriate, clean, dry metal pail lined with plastic, cardboard, aluminum foil or plastic bucket bag, net weight of each piece is generally 25kg. According to user requirements or the order agreement, the use of other forms of packaging, it should comply with the provisions of GB 3796.

5.3 Storage

Gibberellic acid original drug package should be stored in ventilated, cool, dry coffers, fire, moisture, and can not be in the open air with toxic substances, flammable Explosive materials and basic materials stacked together. Not with food, seeds, feed mixed release.

Storage and transportation to prevent moisture and sun, and rain to avoid collision, away from fire.

5.4 Security

This product is a low toxicity plant growth regulator. The FDA should wear protective gloves, masks, wearing clean protective clothing. Not with the use of basic Mixed goods, can not be mixed with ammonia, calcium polysulfide, soda ash and the like. Used with the distribution, once dubbed the aqueous solution can not go far. Immediately after use with Wash water. In case of poisoning, should go to hospital for treatment.

5.5 Acceptance of

Acceptance of gibberellic acid original drug is a month. From the date of delivery, product quality inspection completed within a month, the indicators should meet Combined standards.

Appendix A

(Informative)

Other names gibberellic acid, structural formula and basic physicochemical parameters this product is an active ingredient gibberellic acid is another name, structural formula and basic physicochemical parameters are as follows.

ISO common name. Gibberelicacid CIPAC Numeric Code. 307 CAS Registry Number. 77-06-5 Chemical name. (1alpha, 2beta, 4aalpha, 4bbeta, 10beta) -2,4a, 7- trihydroxy-1-methyl-8-methyl-3-ene-1,10-gibberellic acid -1 , 4a-Lactone Structure.

Empirical formula. C19H22O6 Molecular Weight. 346.4 Biological activity. Plant Growth Regulator Melting point. 223 °C ~ 225 °C (decomposition) Solubility. water 5g/L (room temperature). Soluble in methanol, ethanol, acetone, alkaline aqueous solution, slightly soluble in diethyl ether and ethyl acetate, insoluble Chloroform. Its potassium, sodium, ammonium salts soluble in water (potassium salt 50g/L) Stability. At room temperature in a dry state is stable, slow degradation in aqueous or aqueous alcohol solution in, DT50 (20 °C) about 14d (pH3 ~ 4), 14d (pH7), alkali metal will be converted into less biologically active compounds, the case of thermal decomposition.