GB 22625-2008Prochloraz emulsion, oil in water (English PDF)

3.1 Composition and appearance

This product should be compliant prochloraz original drug with suitable additives formulated, should be a stable liquid, long after a small amount of points allowed Layer, a slight shaking or agitation should be uniform.

3.2 Technical Specifications

Prochloraz water emulsion should meet the requirements of Table 1.

Table 1 prochloraz emulsion in water quality control program indicators

project

index

25% 45% 450g/L

Prochloraz mass fraction a /% or concentration/(g/L) 25.0 + 45.0 + 2.2-2.2 1.5-1.5 2.0-2.0 40.0 + - - + 22-22 450 2,4,6-trichlorophenol mass fraction b /% <= 0.2 0.3 a pH range of 5.5 to 8.5 Pourability After pouring the residue mass fraction /% <= 5.0 After washing the residue mass fraction /% <= 0.5 Emulsion stability (diluted 200 times) Qualified Persistent amount of foam (placed 1min)/mL <= 25 Thermal storage stability test b qualified Low temperature stability test b qualified when a dispute occurs when mass to the mass fraction of arbitration.

B when normal production of 2,4,6-trichlorophenol mass fraction, thermal storage stability test, measuring low temperature stability test at least once every three months.

Test Method 4

4.1 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 1000mL.

4.2 Identification Test

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

4.3 Determination of the mass fraction of prochloraz

4.3.1 Method summary

Sample was dissolved in methanol, acetonitrile + methanol + water as the mobile phase, to use as filler AgilentTC-C18 stainless steel column and ultraviolet Detector (225nm), the sample of prochloraz reverse phase high performance liquid chromatography, external standard. You can also use capillary gas Chromatography, chromatographic operating conditions given in Appendix A.

4.3.2 Reagents and solutions

Methanol. HPLC grade;

Acetonitrile. HPLC grade;

Water. The new secondary steam distilled water;

Prochloraz standard. a known mass fraction >=98.0%.

4.3.3 Instruments

High performance liquid chromatography. a variable wavelength UV detector;

Chromatographic data processor or workstation;

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

Filter. pore size of about 0.45µm;

Micro injector. 50µL;

Quantitative sample line. 5µL;

Ultrasonic cleaner.

4.3.4 HPLC operating conditions

Mobile phase. psi (methanol. acetonitrile. water) = 30.40.30 by membrane filtration, and degassing;

Flow rate. 1.0mL/min;

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

Detection wavelength. 225nm;

Injection volume. 5µL;

Retention time. about 12.0min.

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 prochloraz water emulsion HPLC is shown in Figure 1.

1 --- prochloraz.

Figure 1 prochloraz water emulsion by high performance liquid chromatogram

4.3.5 Measuring step

4.3.5.1 Preparation of standard solution

Weigh 0.1g (accurate to 0.0002g) Prochloraz standard in 50mL volumetric flask, dissolved in methanol and diluted to the mark. use Pipette above solution 10mL in 50mL volumetric flask, diluted with methanol to the mark.

4.3.5.2 Preparation of sample solution

Weigh containing prochloraz 0.1g (accurate to 0.0002g) sample in 50mL volumetric flask, dissolved in methanol and diluted to the mark, shake uniform. Using a pipette to take the above solution 10mL in 50mL volumetric flask, diluted with methanol to the mark.

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 prochloraz 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

Prochloraz sample mass fraction of 1 (%), according to equation (1) calculation; mass density rho1 (g/L), according to equation (2).

1 = A2

rho1 =

10 (2)

Where.

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

A2 --- sample solution, Prochloraz amines mean peak area;

Density rho --- 20 °C when the sample in grams per milliliter (g/mL) (according to GB/T 4472 measured);

--- Prochloraz standard mass fraction, expressed as a percentage.

4.3.7 Allowable difference

Prochloraz mass fraction two parallel determination results relative error should not exceed 2.5%, and the arithmetic mean as a measurement result.

4.4 2,4,6-trichlorophenol mass fraction determination

4.4.1 Method summary

Sample was dissolved in methanol, acetonitrile + water as the mobile phase, to use as filler AgilentTC-C18 stainless steel column and UV detector (215nm), the sample of 2,4,6-trichlorophenol by reverse phase high performance liquid chromatography, external standard.

4.4.2 Reagents and solutions

Acetonitrile. HPLC grade;

Water. The new secondary steam distilled water;

2,4,6-trichlorophenol standard. a known mass fraction >=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 (. I.d) stainless steel column, built AgilentTC-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) = 55.45, by membrane filtration, and degassing;

Flow rate. 1.0mL/min;

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

Detection wavelength. 215nm;

Injection volume. 5µL;

Retention time. about 4.0min.

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 prochloraz water emulsion of 2,4,6-trichlorophenol was measured by HPLC is shown in Figure 2.

1 --- 2,4,6-trichlorophenol;

2 --- prochloraz.

Figure 2 prochloraz water emulsion of 2,4,6-trichlorophenol was measured by high performance liquid chromatogram

4.4.5 Measuring step

4.4.5.1 Preparation of standard solution

Weigh 0.01g (accurate to 0.0002g) 2,4,6- trichlorophenol standard sample in 50mL volumetric flask, dissolved in methanol and diluted to the mark Degree, shake.

4.4.5.2 Preparation of sample solution

Weigh-containing 2,4,6-trichlorophenol 0.01g (accurate to 0.0002g) sample in 50mL volumetric flask, dissolved in methanol and diluted 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 2,4,6-trichlorophenol peak area After the relative change of less than 1.5%, according to the solution, sample solution, sample solution, standard order of standard solution was measured.

4.4.6 Calculation

The two needle sample solution and measured before and after the two doses of the standard sample solution of 2,4,6-trichlorophenol peak areas are averaged. test Samples 2,4,6-trichlorophenol 2 mass fraction (%), according to equation (3) Calculated.

2 = A2

Where.

A1 --- standard solution, the average of 2,4,6-trichlorophenol peak area;

--- The A2 in the sample solution, an average value of the peak area of 2,4,6-trichlorophenol;

--- 2,4,6-trichlorophenol standard mass fraction, expressed as a percentage.

4.4.7 Allowable difference

The relative deviation of two measurements shall be not more than 20% of the arithmetic mean as a measurement result.

According to GB/T 1601 carried out.

4.6 Emulsion stability test

Standard hard water sample was diluted 200-fold, according to GB/T 1603 test, the non-oil slick, no precipitation under qualified.

4.7 Determination of dumping

4.7.1 Method summary

Once placed in a container of water emulsion sample placed certain period of 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.

4.7.2 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).

4.7.3 Test procedure

Mix well enough samples, some of which have been promptly placed weighed measuring cylinder (including plug), attached to 8/10 of the cylinder, the plug Tight grinding mouth stuffed, place the determined time (24h). The tap is opened, the upright position of the rotating cylinder by a 135 ° angle of dumping 60s, then invert 60s, heavy the new weighing cylinder and a stopper.

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 weighing cylinder and a stopper.

4.7.4 Calculation

Mix well after pouring a sufficient amount of sample residue mass fraction of 3 residue mass (%) and after washing fraction 4 (%), respectively, according to the formula (4) and (5) Calculated.

100 (4)

100 (5)

Where.

4.8 Determination of the amount of long-lasting foam

4.8.1 Method summary

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

4.8.2 Reagents and solutions

Standard hard water. rho (Ca 2 ++ Mg2 +) = 342mg/L, pH = 6.0 ~ 7.0. According to GB/T 14825 preparation.

4.8.3 Instruments and Appliances

Stoppered cylinder. 250mL (division value 2mL, 0 ~ 250mL tick 20cm ~ 21.5cm, 250mL scale line to the bottom plug 4cm ~ 6cm);

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

4.8.4 Measuring step

The cylinder is added to 180mL standard hard water scale line at set cylinder on balance, weighed into the sample 1.0g (accurate to 0.1g), plus standard Hard water from the bottom of the cylinder to the mark at 9cm, the cover plug for the bottom of the cylinder as the center, upside down 30 times (2s). On trial Test bench standing 1min, record lather volume.

4.9 Thermal storage stability test

According to GB/T 19136 in "liquid formulation" to. Thermal storage after prochloraz content should be not less than 95% before the thermal storage, other indicators should Meet the requirements of this standard is qualified.

4.10 Low temperature stability test

According to GB/T 19137 in "homogeneous emulsion and liquid preparations", in the bottom of the centrifuge tube educt volume does not exceed 0.3mL qualified.

4.11 Product inspection and acceptance

Product inspection and acceptance shall comply with GB/T 1604's. Treatment of extreme values, using the rounding value comparison method.