Medical grade menthol oil experiment application research and development test

Medical grade menthol oil experiment declared the development of small test menthol oil Bohesu YouPEPPERMINT OIL This product is a volatile oil
extracted by water vapor distillation, freezing and partial debrainization of the fresh stems and leaves of the lip family plant Mentha haplocalyx Briq.
【Properties】This product is a colorless or yellowish clear liquid; It has a special cool aroma, the taste is first spicy, and then cool
.
After storing for a long time, the color gradually becomes darker
.
This product and ethanol can be arbitrarily miscinct
.
The relative density should be 0.
888~0.
908 (General 0601).

Optical rotation Take this product, determined according to law (general rule 0621), the optical rotation should be -17 ° ~ -24 °
.
The refractive index should be 1.
456 to 1.
466 (general rule 0622
).
【Identification】Take 0.
1g of this product, add 5ml of absolute ethanol to dissolve, as a solution
for the test.
Another menthol oil control extract is taken and the control extract solution
is made by the same method.
According to the thin layer chromatography (General Rule 0502) test, aspirate 5 μl of each of the above two solutions, respectively, on the same silica gel GF254 thin layer plate, with toluene-ethyl acetate (19:1) as the unfolding agent, unfold, remove, dry, placed under a UV lamp (254nm) for inspection
.
In the chromatography of the test product, spots
of the same color are shown at the corresponding position as the control extract chromatography.
Spray with anise-aldehyde test solution and heat at 105 °C until the spots are clearly
colored.
In the chromatography of the test product, spots of the same color are shown at the corresponding position as the control extract chromatography; Examine under a UV lamp (365 nm) to show fluorescent spots
of the same color.
【Check】Color Take this product and the same volume of yellow No.
6 standard colorimetric solution, not deeper
.
Insoluble matter in ethanol Take 1ml of this product, add 70% ethanol 3.
5ml, the solution should be clarified
.
The acid number should not be greater than 1.
5 (General 0713
).
【Fingerprint】Measured
by gas chromatography (General Rule 0521).
Chromatography conditions and system suitability test Capillary column with modified polyethylene glycol as the fixed phase (column length of 30m, inner diameter of 0.
25mm, film thickness of 0.
25μm); column temperature as the programmed heating: initial temperature of 60 °C, maintained for 4 minutes, heating at a rate of 1.
5 °C per minute to 130 °C, and then heating at 20 °C per minute to 200 °C; inlet temperature 250 °C; detector temperature 250 °C; shunt injection, shunt ratio 100:1
.
The theoretical number of plates should not be less than 50,000 according to the mint peak
.
Preparation of reference solution Take eucalyptus oil essence control, (a) - menthol control, menthol control, precision weighing, respectively, add absolute ethanol to make a solution containing 5mg per 1ml, that is, obtained
.
Preparation of the solution for the test product Take this product, that is, obtained
.
Determination method Respectively, accurately aspirate 2μl of the reference solution and 0.
2μl of the test solution, inject into the gas chromatograph, measure, record the chromatogram, that is, obtain
.
Control fingerprint peak S1: eucalyptus peak S2: (a) - mentholone peak peak S3: menthol The fingerprint of the test product should be presented with the same chromatographic peak retention time as the reference object chromatographic peak, calculated according to the Chinese herbal chromatography fingerprint similarity evaluation system, the similarity between the fingerprint of the test product and the control fingerprint should not be less than 0.
90
.
Integral parameters Slope sensitivity is 1, peak width is 0.
1, minimum peak area is 20, and minimum peak height is 10
.
【Content determination】Determination
by gas chromatography (General Rule 0521).
Chromatography conditions and system suitability test Capillary column with modified polyethylene glycol as the fixed phase (column length of 30m, inner diameter of 0.
25mm, film thickness of 0.
25μm); column temperature as the programmed heating: initial temperature of 60 °C, maintained for 4 minutes, heated to 100 °C at a rate of 2 °C per minute, and then heated to 230 °C per minute to 230 °C for 1 minute; inlet temperature 250 °C; detector temperature 250 °C; shunt injection, shunt ratio 5:1
.
The number of theoretical plates should not be less than 20,000 according to the naphthalene peak
.
Correction factor determination Take the appropriate amount of naphthalene, weigh it precisely, add absolute ethanol to make a solution containing 1.
8mg per 1ml, shake well, as an internal standard solution
.
Another menthol control is about 30mg, precision weighing, placed in a 10ml measuring flask, add the internal standard solution to the scale, shake well, pipette 1 μl into the gas chromatograph, calculate the correction factor
.
Determination method Take about 80mg of this product, weigh it precisely, place it in a 10ml measuring flask, add the internal standard solution to the scale, shake well, suck 1μl into the gas chromatograph, measure, that is, obtain
.
This product contains menthol (C10H20O) should be 28.
0% to 40.
0%.

【Storage】Shading, sealing, placed in a cool place
.