Pharmaceutical grade betaclodextrin experiment declaration research and development test

Pharmaceutical grade betacyclodextrin experimental declaration of research and development of small test pH Take 0.
20g of this product, add 20ml of water to dissolve, add saturated solution 0.
2ml, measured according to law (Appendix VI.
H), pH value should be 5.
0-8.
0
.

The clarity and color of the solution Take 0.
50g of this product, add 50ml of water to dissolve, the solution should be clear and colorless; if it is cloudy, compared with the No.
2 turbidity standard (Appendix IX.
B), it should not be more concentrated
.

Chloride Take 0.
39g of this product, check according to law (Appendix VIII.
A), and compare with the control solution made of standard sodium chloride solution of 7.
0ml, no more concentrated (0.
018%)
.

Impurity absorbance Take about 1g of this product, precision weighing, add 100ml of water solvent, according to ultraviolet - visible spectrophotometry determination, absorbance in the wavelength range of 230-250 nm shall not exceed 0.
1, absorbance in the wavelength range of 350-750 nm shall not exceed 0.
05.
reducing sugar Take this product 1.
0g, precision weighing, add 25ml of water to dissolve, add alkaline copper tartarate test solution 40ml, slowly boil for 3 minutes, room temperature overnight, filter with G4 vertical molten funnel, precipitate with warm water until the lotion is neutral, discard the filtrate and lotion, precipitate with hot iron sulfate test solution 20ml dissolved, filtered, filtered, filtered with water 100ml wash, combined filtrate and lotion, heated to 60 ° C, titrated with potassium permanganate titration solution (0.
02mol/L) while hot
.

According to the calculation of dried products, the consumption of potassium per 1 g of potassium per 1 g (0.
02 mol/L) shall not exceed 3.
2 ml (1.
0%)
.

Cyclohexane Take about 0.
2g of this product, precisely weighed, placed in the top empty bottle, add the internal standard solution (take an appropriate amount of dichloroethylene, add 20% dimethyl sulfoxide solution to make a solution containing about 0.
04 μg per 1ml, that is) 10.
0ml, as a test solution; another precision called cyclohexane, add the internal standard solution to make a solution containing about 0.
078mg of cyclohexane per 1ml, and take 10.
0ml of empty bottle as a control solution
.

According to the residual solvent assay (Appendix VIII.
P) test, the capillary column with 100% dimethicone as the fixative solution is the column; The column temperature is 90 °C; The inlet temperature is 200 °C; Detector temperature is 250 °C; The equilibration temperature of the head empty bottle is 70 °C, and the equilibration time is 20 minutes
.

Take the headspace injection of the control solution, and the degree of separation between the peaks of each component should comply with the regulations
.

Take the sample solution and the control solution to inject the headspace respectively, record the chromatogram, and calculate the peak area according to the internal standard method, which should comply with the regulations
.