GB 22612-2008Cartap hydrochloride technical (English PDF)

3.1 Appearance

White powder or white crystals.

3.2 Technical Specifications

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

Table 1 CARTAP original drug control project indicators

Item Index

CARTAP mass fraction /% >= 97.0 Moisture content /% <= 1.0 Score a /% Water insoluble mass <= 0.2 pH range 3.0 to 6.0 when a normal production, the quality of water insoluble fraction was measured 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. Determined by sampling a random number table method packages, the final sample size not less than 100g.

4.2 Identification Test

You can choose one of the following methods. When not identify one way, then use another method should be determined.

Infrared spectroscopy --- CARTAP sample and standard samples in the infrared 4000cm-1 ~ 400cm-1 absorption spectrum should be no significant difference.

CARTAP standard infrared spectrum is shown in Figure 1.

Figure 1 CARTAP standard infrared spectrum

HPLC --- The identification test can be carried out simultaneously with the determination of the mass fraction of CARTAP. In the same chromatographic operating conditions , The sample solution to a chromatographic retention time and CARTAP CARTAP standard solution peak retention time, the relative difference should 1.5% or less.

Determination of the mass fraction of 4.3 CARTAP

4.3.1 Method summary

Phosphoric acid aqueous sample was dissolved in heptane solution of sodium + acetonitrile as mobile phase, to use as filler Capcel-PakC18 stainless steel Column and UV detector (225nm), the sample of CARTAP reverse phase high performance liquid chromatography, external standard.

4.3.2 Reagents and solutions

Acetonitrile. HPLC grade;

Water. The new secondary steam distilled water;

Phosphoric acid;

Phosphoric acid. water with phosphoric acid adjusted to pH 2.5;

Geng sodium;

Triethylamine;

Heptane sulfonate solution. Weigh 3.64g of sodium heptanoate in 1L wide-mouth bottle, add distilled water 900mL secondary shaking to dissolve, Phosphoric acid was added 16mL; then triethylamine adjusted to pH 2.0;

CARTAP standard. a known mass fraction >=99.0%.

4.3.3 Instruments

High performance liquid chromatography. a variable wavelength UV detector;

Chromatographic data processor or chromatography workstation;

Column.200mm × 4.6mm (. I.d) stainless steel column, built Capcel-PakC18,5µm filler (or with equivalent effect color the column);

Filter. pore size of about 0.45µm;

Micro injector. 50µL;

Quantitative sample line. 10µL;

Ultrasonic cleaner.

4.3.4 HPLC operating conditions

Mobile phase. psi (heptane solution of sodium. acetonitrile) = 90.10, with 0.45µm filter membrane, ultrasound 10min spare;

Flow rate. 1.0mL/min;

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

Detection wavelength. 225nm;

Injection volume. 10µL;

Retention time. 7.4min.

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 CARTAP original drug HPLC is shown in Figure 2.

1 --- CARTAP.

HPLC Figure 2 CARTAP original drug

4.3.5 Measuring step

4.3.5.1 Preparation of standard solution

Weigh 0.05g (accurate to 0.0002g) CARTAP standard, a 50mL volumetric flask, dissolved in aqueous phosphoric acid and diluted to the mark Degree, shake.

4.3.5.2 Preparation of sample solution

Weigh containing CARTAP 0.05g (accurate to 0.0002g) sample, placed in 50mL volumetric flask, and diluted with aqueous phosphoric acid 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 fenitrothion Danfeng area relative change After less than 1.5%, according to the solution, sample solution, sample solution, standard order of standard solution was measured.

4.3.5.4 Calculation

The two needle sample solution and measured before and after the two doses of the standard sample solution fenitrothion Danfeng area were averaged. Sample CARTAP the mass fraction of 1 (%) according to equation (1).

1 = A2

Where.

A1 --- standard solution, fenitrothion mean Danfeng area;

A2 --- sample solution, fenitrothion mean Danfeng area;

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

4.3.6 Allowable difference

CARTAP poor quality score of two parallel determination results shall not be greater than 1.2%, the arithmetic mean value as a measurement result.

4.4 Determination of Moisture

According to GB/T 1600 in "azeotropic method".

4.5 Determination of insoluble matter

4.5.1 Reagents and Instruments

Conical flask. 250mL;

Glass sand core crucible. G3;

Oven. 105 °C ± 2 °C;

Suction flask. 500mL.

4.5.2 Determination

Weigh 10g sample (accurate to 0.01g), into a conical flask, 100mL water, shaking the sample has been dissolved immediately by Constant weight (accurate to 0.0002g) filter crucible, and then 60mL of water, washed three times Erlenmeyer flask filtration. The crucible was placed in an oven dried 2h, brought out in the dryer to cool and weigh (accurate to 0.0002g).

4.5.3 Calculation

Sample water insolubles 2 (%) according to equation (2).

Where.

4.5.4 Allowable difference

Relative deviation parallel determination results shall be not more than 30% of the arithmetic mean as a measurement result.

According to GB/T 1601 carried out.

4.7 Product testing and acceptance

Shall comply with GB/T 1604 regulations limit the use of numerical processing rounding value comparison method.