Pharmaceutical grade carbomer 940 carbomer homopolymer spot pharmacopoeia standard

Pharmaceutical grade carbomer 940 carbomer homopolymer spot pharmacopoeia standard residual solvent ethyl acetate and cyclohexane (determined when used in the production process) Take about 0.
2g of this product, precision weighing, placed in a headspace bottle, precision addition of dimethyl sulfoxide 5ml, sealed, as a test solution; respectively, take ethyl acetate and cyclohexane appropriate amount, precision weighing, with dimethyl sulfoxide quantitative dilution into each 1ml containing ethyl acetate 0.
2mg and cyclohexane 0.
12mg mixed solution, precision dose 5ml, placed in a headspace bottle, sealed, as a control solution
.

According to the residual solvent assay (general rule 0861 second method), with 100% dimethyl polysiloxane (or similar polarity) as the fixed liquid capillary column, programmed heating, starting temperature of 40 °C, maintained for 3 minutes, at a rate of 5 °C per minute to 120 °C, maintained for 20 minutes, and then at a rate of 20 °C per minute to 220 °C, maintained for 3 minutes, and then at a rate of 20 °C per minute to 240 °C, maintained for 8 minutes; Inlet temperature 260°C; Detector temperature 260°C; The equilibrium temperature of the headspace bottle is 85 ° C and the equilibration time is 90 minutes
.

Take the control solution and the test solution respectively headspace injection
.

According to the external standard method based on the peak area, the content of ethyl acetate shall not exceed 0.
5%, and cyclohexane shall not exceed 0.
3%.
Benzene take the appropriate amount of benzene, precision weighing, with dimethyl sulfoxide quantitative dilution made of each 1ml of benzene 1.
0mg solution, precision amount of appropriate amount, quantitative dilution of water to make a solution containing 0.
5μg of benzene per 1ml, as benzene storage solution
.

Take this product about 250mg, precision weighing, placed in a headspace bottle, precision addition of 2% sodium chloride solution 10.
0ml, mechanical mixing (about 30 minutes), sealed, as a test solution, this solution should be sampled within 3 hours after preparation; take this product about 250mg, precision weighing, placed in a headspace bottle, precision addition of 2% Sodium chloride solution 9.
0ml, mechanically mixed homogeneously (about 30 minutes), precision added benzene stock solution 1ml, mechanically mixed evenly (about 1 min), sealed, as a control solution
.

According to the residual solvent determination method (general rule 0861 second method), with 6% cyanopropyl phenyl -94% dimethyl polysiloxane as the fixed liquid capillary column, programmed heating, starting temperature of 40 °C, maintained for 20 minutes, at a rate of 10 °C per minute to 240 °C, maintained for 20 minutes; The inlet temperature is 140 °C, the detector is a hydrogen flame ionization detector, the temperature is 250 °C; The equilibrium temperature of the headspace bottle is 80 °C, the equilibration time is 60 minutes, and the headspace is filled
.

Taking the control solution as the system suitability solution, the chromatographic peak height of benzene should be more than 10 times the baseline noise, and the relative standard deviation of the peak area of benzene should not exceed 15%
if injected three times continuously.

Take the control solution and the test solution respectively headspace injection, the peak area of benzene in the test solution shall not be greater than half of the peak area of benzene in the control solution (0.
0002%)
.