Medical grade phenoxyethanol experiment declaration research and development test

Medical grade phenoxyethanol experiment declaration research and development of small test phenoxyethanol BenyangyichunPhenoxyethanol This product is 2-phenoxyethanol
.
The content of C8H10O2 should be 98.
0%~102.
0%.

【Properties】This product is a colorless and slightly viscous liquid
.
This product is arbitrarily miscible with acetone, ethanol or glycerol, and slightly soluble
in water.
Relative density The relative density of this product (General 0601) is 1.
105~1.
110
.
Refractive index The refractive index of this product (General 0622) is 1.
537~1.
539
.
【Identification】(1) In the chromatogram recorded under the content determination item, the retention time of the main peak of the test solution should be consistent
with the retention time of the main peak of the reference solution.
(2) take this product, weigh it accurately, add water to dissolve and quantitatively dilute to make a solution containing about 80μg per 1ml, determined by ultraviolet-visible spectrophotometry (General 0401), with maximum absorption
at 269nm and 275nm wavelengths.
The absorption coefficient at the wavelength of 269nm is 95~105, and the absorption coefficient at the wavelength of 275nm is 75~85
.
(3) The infrared light absorption spectrum of this product should be consistent with the spectrum of the reference substance (General rule 0402).

【Inspection】Related substances take an appropriate amount of this product, weigh it accurately, add absolute ethanol to dissolve and quantitatively dilute to make a solution containing about 250mg per 1ml, shake well, and use it as a test solution; Take an appropriate amount with precision and dilute it with absolute ethanol to make a solution containing about 0.
25mg per 1ml as a control solution
.
According to the chromatographic conditions under the content determination item, 1μl of the test solution and 1μl of the control solution were accurately measured, injected into the gas chromatograph respectively, and the chromatogram was
recorded.
If there are impurity peaks in the chromatogram of the test solution, the peak area of a single impurity shall not be greater than the peak area of the main peak in the control solution (0.
10%); The sum of the peak areas of each impurity shall not be greater than 3 times (0.
3%)
of the main peak area in the control solution.
The chromatographic peaks in the chromatogram of the test solution that are less than 0.
5 times (0.
05%) of the main peak area of the control solution are ignored
.
Ethylene oxide and dioxane take 1g of this product, weigh it accurately, put it in an empty bottle, and add N accurately, N-dimethylacetamide 1.
0ml and water 0.
2ml, sealed, shaken, as a test solution; precision take an appropriate amount of ethylene oxide aqueous solution reference substance, dilute with water to make a solution containing about 10μg per 1ml, as an ethylene oxide reference solution; take an appropriate amount of dioxane hexacycline, precision weighing, add water to quantitatively dilute to make a solution containing 0.
5mg per 1ml, as a dioxane reference solution; take 1g of this product, weigh it accurately, put it in an empty bottle, add 1.
0ml of N,N-dimethylacetamide accurately, 0.
1ml of ethylene oxide reference solution and 0.
1ml of dioxane reference solution, seal, shake well , as a reference solution; Take 0.
1ml of ethylene oxide reference solution, put it in an empty bottle, add 0.
1ml of freshly prepared 0.
001% acetaldehyde solution and 0.
1ml of dioxane reference solution, seal, shake well, and use it as a system suitability test solution
。 According to gas chromatography (General 0521), a capillary column with 5% diphenyl-95% dimethylsiloxane (or similar polarity) as the stationary solution is used as the column, the starting temperature is 32 °C, maintained for 5 minutes, heated to 180 °C at a rate of 5 °C per minute, and then heated to 230 °C at a rate of 30 °C per minute, maintained for 5 minutes (can be adjusted according to specific conditions).

The inlet temperature is 150°C, the detector is a hydrogen flame ionization detector with a detector temperature of 250°C, and the equilibration temperature of the headspace bottle is 70°C, and the equilibration time is 45 minutes
.
Take the headspace injection of the system suitability test solution, the resolution between the acetaldehyde peak and the ethylene oxide peak should not be less than 2.
0, and the height of the dioxane peak should be more than
5 times the baseline noise.
The relative standard deviation of the ethylene oxide peak area shall not exceed 15% and the relative standard deviation of the dioxane peak area shall not exceed 10%
in at least 3 repeat injections.
The headspace injection of the test solution and the reference solution were taken respectively, and according to the standard addition method, ethylene oxide shall not exceed 0.
0001%, and dioxane shall not exceed 0.
001%.

【Content determination】Determined
by gas chromatography (General 0521).
Chromatographic conditions and system suitability test The quartz capillary column with polyethylene glycol 20M (or similar polarity) as the stationary solution is the column, the starting column temperature is 90 °C, the temperature is raised to 220 °C at a rate of 10 °C per minute, maintained for 10 minutes, the inlet temperature is 250 °C, the detector temperature is 270 °C, and the split ratio is 1:100
.
take an appropriate amount of this product and phenol, add absolute ethanol to dissolve and dilute to make a solution containing about 0.
25mg per 1ml, take 1μl into the gas chromatograph, record the chromatogram, the resolution of phenol peak and phenoxyethanol peak should not be less than 15.
0
.
Determination method take an appropriate amount of this product, weigh it accurately, add absolute ethanol to dissolve and quantitatively dilute to make a solution containing 5mg per 1ml, as a test solution, take 1μl of precision and inject it into the gas chromatograph, and record the chromatogram; In addition, phenoxyethanol reference substance was taken, precision weighed, and determined
by the same method.
According to the external standard method, the peak area is calculated, that is, obtained
.
【Category】Pharmaceutical excipients, bacteriostatic agents
.
【Storage】Protect from light, sealed and preserved
.