GB 22623-2008Prochloraz technical (English PDF)

3.1 Appearance

Light yellow to brown viscous liquid, cooled and solidified.

3.2 Technical Specifications

Prochloraz original drug should also meet the requirements of Table 1.

Table 1 prochloraz original drug control project indicators

Item Index

Prochloraz mass fraction /% >= 95.0 2,4,6-trichlorophenol mass fraction a /% <= 0.5 A mass acetone insoluble fraction /% <= 0.2 Moisture content /% <= 0.5 a pH range of 5.5 to 8.5 a normal production acetone insoluble, 2,4,6-trichlorophenol is determined at least once every three months.

Test Method 4

4.1 Sampling

According to GB/T 1605-2001 "on the original drug product sampling" approach. Determining sample package using a random number table method; the final sample size not less than 100g.

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.

Infrared spectroscopy --- sample and standard prochloraz in the range 4000cm-1 ~ 400cm-1 infrared absorption spectrum should be no significant area do not. Prochloraz standard infrared spectrum is shown in Figure 1.

Figure 1 prochloraz standard infrared spectrum

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, operating conditions, see 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 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.

4.3.4 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 original drug HPLC is shown in Figure 2.

1 --- prochloraz.

Figure 2 HPLC prochloraz original drug

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

The two needle sample solution and measured before and after the two doses of the standard sample solution PROCHLORAZ peak areas are averaged. Sample PROCHLORAZ the mass fraction of 1 (%), according to equation (1).

1 = A2

Where.

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

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

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

4.3.7 Allowable difference

Prochloraz difference between an amine content of two parallel determination results shall not be greater than 1.5%, the arithmetic mean value 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 original drug 2,4,6-trichlorophenol measured by HPLC is shown in Figure 3.

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

2 --- prochloraz.

Figure 3 prochloraz original drug 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 (2).

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.

4.5 Determination of acetone insolubles

According to GB/T 19138 performed.

4.6 Determination of Moisture

According to GB/T 1600 the "Karl Fischer method".

According to GB/T 1601 carried out.

4.8 Product testing and acceptance

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