GB 28138-2011Mesotrione aqueous suspension concentrate (English PDF)

3.1 Composition and appearance

This product should be compliant mesotrione original medicines, additives and fillers processed and should be mobile, easy to measure the volume of the liquid suspension, Precipitation may occur during storage, handling but shaken, restitution should, there should be no lumps.

3.2 Technical Specifications

Mesotrione suspensions shall comply with the requirements in Table 1.

Table 1 mesotrione SC Control Project Index

project

index

10% 15%

Mesotrione mass fraction /% 10.0 15.0 0.9-0.9 0.9-0.9 Suspension rate /% >= 90 pH range 3.0 to 6.0

Table 1 (continued)

project

index

10% 15%

Pourability

After pouring the residue /% <= 5.0 After washing the residue /% <= 0.5 Wet sieve test (through 75µm test sieve) /% >= 98 Persistent foaming (foam volume after 1min)/mL <= 30 Low temperature stability a qualified Thermal storage stability of a qualified Low temperature stability test, thermal storage stability test was measured at least once every three months during a normal production.

Test Method 4

Safety Tips. Use of this standard shall have practical experience of laboratory personnel work. This standard does not point out all of the safety issues. Make with those who have the responsibility to take appropriate safety and health practices and to ensure compliance with the relevant national regulations.

4.1 General provisions

This standard reagents and water in the absence of other requirements specified, refers to three analytical reagent and GB/T 6682-2008 specified in water. Test results determined in accordance with GB/T 8170-2008 4.3.3 Rounding the value comparison method.

4.2 Sampling

According to GB/T 1605-2001 in "liquid formulations sampling" approach. Determining sample package using a random number table method; the final sample size not less than 600mL.

4.3 Identification Test

Liquid chromatography --- The identification test can be carried out simultaneously with the determination of mesotrione mass fraction. Under the same chromatographic operating conditions, Retention time of the sample solution and the standard solution to a peak of mesotrione retention time peaks, the relative difference should be 1.5% Fewer.

4.4 Determination of mesotrione mass fraction

4.4.1 Method summary

Sample dissolved in mobile phase acetonitrile water (adjusted with phosphoric acid to pH 3) as the mobile phase, C18 to use as filler and a stainless steel column UV detector at a wavelength of 270nm, the sample of mesotrione reverse phase HPLC separation and determination of external standard.

4.4.2 Reagents and solutions

Acetonitrile. HPLC grade;

Water. The new secondary steam distilled water;

Phosphoric acid;

Mesotrione standard. a known mass fraction w>=99.0%.

4.4.3 Instruments

High performance liquid chromatography. a variable wavelength UV detector;

Chromatographic data processor or chromatography workstation;

Column. 250mm × 4.6mm (id) stainless steel column, built C18,5µm filler (or with equivalent effect column);

Filter. pore size of about 0.45µm;

Micro injector. 50µL;

Quantitative sample line. 5µL;

Ultrasonic cleaner.

4.4.4 HPLC operating conditions

Mobile phase. [Psi] [acetonitrile. water (adjusted with phosphoric acid to pH 3)] = 40.60, filtered through a filter membrane and degassed;

Flow rate. 1.0mL/min;

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

Detection wavelength. 270nm;

Injection volume. 5µL;

Retention time. mesotrione about 10.1min.

It said operating parameters are typical, according to the characteristics of different instruments, given operating parameters adjusted as appropriate, in order to obtain the best results.

Typical mesotrione SC HPLC is shown in Figure 1.

1 --- mesotrione.

Figure 1 mesotrione suspending HPLC Fig.

4.4.5 Measuring step

4.4.5.1 Preparation of standard solution

Weigh 0.1g (accurate to 0.0002g) mesotrione standard sample in 50mL volumetric flask with acetonitrile to volume, ultrasonic oscillation 5min make sample dissolution, cooled to room temperature and shake well. Using a pipette to take the above solution 5mL to 50mL volumetric flask, dilute with mobile phase to the mark.

4.4.5.2 Preparation of sample solution

Weigh containing mesotrione 0.1g (accurate to 0.0002g) sample in 50mL volumetric flask with acetonitrile to volume, ultrasonic transducer Swing 5min, cooled to room temperature, shaken and filtered. Using a pipette to take the above solution 5mL to 50mL volumetric flask, dilute with mobile phase to Mark and shake.

4.4.5.3 Determination

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

4.4.5.4 Calculation

The two needle sample solution and measured before and after the two doses of the standard sample solution mesotrione peak areas are averaged. Mesotrione sample Grass-one content according to formula (1).

w1 = A2

· M1 · w

A1 · m2

Where.

w1 --- mesotrione sample mass fraction;

A2 --- sample solution, mesotrione mean one peak area;

m1 --- mesotrione standard mass in grams (g);

w --- mesotrione standard mass fraction;

A1 --- the standard solution, the average mesotrione peak area;

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

4.4.6 Allowable difference

Results relative deviation scores twice mesotrione quality parallel determination should not exceed 4% of the arithmetic mean as a measurement result.

Determination of 4.5 pH value According to GB/T 1601 carried out.

4.6 Determination of the suspension rate

According to GB/T 14825-2006 of 4.2. Weigh mesotrione sample containing 0.1g of (accurate to 0.0002g), the remaining 1/10 suspension and precipitate transferred to a 100mL flask with 60mL acetonitrile three times to wash all the residue 25mL 100mL flask, under ultrasonic oscillations 5min, cooled to room temperature, constant volume, shake, filtration, measuring 4.4 by mesotrione quality Calculate the amount of its suspension rate.

4.7 Wet sieve test

According to GB/T 16150 in the "wet sieve method".

4.8 Determination of dumping

4.8.1 Method summary

Will be placed in the container suspending sample placed after a certain time, in accordance with prescribed procedures dumping determined trapped in the sample container Volume; the vessel was washed with water, and then measuring the amount of container.

4.8.2 Instruments

With ground joint stopper cylinder. 500mL ± 2mL; cylinder height 39cm, between the upper and lower scale distance 25mL (or equivalent for the determination of dumping Down of other containers).

4.8.3 Test procedure

Mix well enough samples, some of which have been promptly placed weighed measuring cylinder (including plug) (accurate to 0.01g), attached to the 8/10 of the cylinder, the mill plugged gag, placing a determined time (24h). The tap is opened, the upright position of the rotating cylinder by a 135 ° dumping 60s, Then invert 60s, re-weighing and measuring cylinder plug (accurate to 0.01g).

Would be equivalent to 80% of the cylinder volume of water (20 °C) was poured into a measuring cylinder, stoppered plug grinding mouth, the cylinder upside down 10 times, according to the above tilting operation Pour the contents of the third and weighing cylinder plug (accurate to 0.01g).

4.8.4 Calculation

Mass fraction and mass fraction of residue after washing the sample after pouring the residue, respectively according to formula (2) and (3) Calculated.

w2 = m2-m0m1-m0 ×

100 (2)

w3 = m3-m0m1-m0 ×

100 (3)

Where.

Mass fraction w2 --- sample after pouring the residue, expressed in%;

Mass fraction w3 --- sample after washing residue, expressed in%;

After m2 --- dumping, quality cylinder, grinding gag and residue, in grams (g);

m0 --- cylinder, quality is more important after grinding gag constant in units of grams (g);

m1 --- cylinder, grinding gag and quality of the sample, in grams (g);

--- Washing m3, the quality of the cylinder, grinding gag and residue, in grams (g).

4.9 Determination of Persistent foaming

4.9.1 Method summary

The sample was mixed with a predetermined amount of standard hard water, after standing foam volume recorded.

4.9.2 Reagents

Standard hard water. rho (Ca2 Mg2) = 342mg/L, pH = 6.0 ~ 7.0, according to GB/T 14825-2006 formulated.

4.9.3 Instruments and Appliances

Stoppered cylinder. 250mL (division value 2mL, 0 ~ 250mL tick 20cm ~ 21.5cm, 250mL scale line to the bottom of the plug;

4cm ~ 6cm);

Industrial scale. a sense of the amount of 0.1g.

4.9.4 Measuring step

Added 180mL graduated cylinder standard hard water, 1.0g sample was weighed into a graduated cylinder (accurate to 0.1g), added to standard hard water from the cylinder Plug at the bottom tick 9cm, the cover plug to the bottom of the cylinder as the center, upside down 30 times (2s). Stand on the test stand 1min, record lather volume.

4.10 Low temperature stability test

According to GB/T 19137 in "suspended preparations" in wet sieve test still meet the standards for qualified.

4.11 Thermal storage stability test

According to GB/T 19136 "other agents" to. After the heat storage mesotrione content should not be less than 95% of the reservoir before the suspension was still to be Meet the standards for qualified.

4.12 Product inspection and acceptance

Shall comply with GB/T 1604's.

5.1 Marking, labeling, packaging

Mesotrione suspending marking, labeling and packaging should comply with the provisions of GB 3796. Mesotrione suspending application of PET bottle packaging, each bottled net content is generally 50g, 100g, 250g, 400g. You can also use other forms of packaging according to user requirements or the order agreement, subject to Comply with the provisions of GB 3796.

5.2 Storage

Mesotrione suspension package should be stored in well-ventilated, dry coffers. Storage and transportation, to prevent moisture and sunlight, no food, seed Child, feed-mixing, avoid contact with skin, eyes, mouth and nose to prevent inhalation.

5.3 Security

This product is a low-toxicity herbicides. Wear protective goggles and rubber gloves to wear the necessary protective clothing when using this product. After application with soap and Rinse with water. Coverage should be immediately sent to hospital symptomatic treatment.

5.4 Warranty Period

Under the specified storage conditions, warranties of mesotrione suspension of two years starting from the date of manufacture.

Appendix A

(Informative)

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

ISO common name. Mesotrione CAS Registry Number. 104206-82-8 Chemical Name. 2- (4-methanesulfonyl-2-nitrobenzoyl) cyclohexane-1,3-dione Structure.

Empirical formula. C14H13NO7S Molecular Weight. 339.3 Biological activity. weeding Melting point. 148.7 °C ~ 152.5 °C Solubility (20 °C, g/L). water 0.16mg/L; 1.4-xylene, toluene, 2.7, 3.6 of methanol, acetone, 76.4, 82.7 methylene chloride, Acetonitrile 96.1 Stability. stable water pH5 ~ 9, the original drug 14d storage stability properties 54 °C.