The solvent peak presented is complex, and the choice of 3.2 extraction solvent is first selected according to the swelling and pain aerosol quality specification (for trial). The menthol peak was not able to reach baseline separation. Considering that the liquid contains ethanol, 40% 60% 80% 90% and absolute ethanol are selected as solvents. The result is that the menthol peak can reach baseline separation when anhydrous ethanol is used as a solvent. And the internal standard naphthalene is easily dissolved in absolute ethanol. Through systematic research and methodological verification, the above method is superior to the original method. This method has the advantages of simple pretreatment, sensitivity and accuracy, and provides a more scientific basis for its quality control.

OBJECTIVE: To establish a gas chromatographic method for the determination of menthol in the swelling and pain aerosol. METHODS: The chromatographic conditions were 1909IJ-413HP-5 quartz capillary column. The new drug swelling and pain aerosol consisted of Qiyelian, Sanqi, Xuezhi, and menthol. Gas chromatograph conditions: sequential heating, column temperature 60 ° C, adhere to 5 ° per minute at a temperature increase rate of 5 ° C to 100 ° C, adhere to 2 min split ratio of 251 FID detector, the internal standard is naphthalene. RESULTS: The menthol concentration was linear in the range of 0.01 mg/ml mg/ml (r=0.9998. The average recovery was 101.70%. The RSD was 2.08% n=5. Conclusion: This method is simple in pretreatment, high in sensitivity, and wide in linear range. The separation effect is good and the result is accurate and reliable.

It has significant effects on bruises, periarthritis of shoulder, gout, rheumatoid arthralgia and lobular hyperplasia of the breast. In the trial specification, the content of menthol was determined by gas chromatography, and the pretreatment method was complicated and the time was long. This paper conducted a re-study on the method for determining the content of menthol, and the results are as follows.

1 instruments and reagents

Including hydrogen flame ionization detector; 7683 fully automatic injector; column: 1909IJ-413HP-5 quartz capillary column. Menthol reference substance (batch number 0728-200005 provided by China National Institute for the Control of Pharmaceutical and Biological Products; swollen pain aerosol (batch number 20040126 provided by Yunnan Pharmaceutical Institute Pharmaceutical Factory; the reagents and reagents used are of analytical grade. Agilent, USA 6890) Gas chromatograph system.

2 methods and results

The detector temperature was 250 ° C, and the 2.1 chromatographic conditions selected the inlet temperature to be 250 ° C. The splitting ratio was 251 column temperature 60 ° C, and the temperature was raised to 100 ° C at 5 ° C per minute for 5 min, and the system condition for measuring menthol was determined for 2 min.

Take the reference solution, the internal standard naphthalene solution, and the test solution for injection in 1 μl. The separation of the tested components was better, and the 2.2 system suitability experiment was carried out according to the chromatographic conditions in 2.1. Menthol is separated by baseline, and the number of theoretical plates is greater than 120,000 according to the menthol peak.

Dilute to the mark with absolute ethanol; draw 1.0μl into the gas chromatograph for measurement, 2.3 linear relationship, accurately weigh the menthol reference substance 57.07mg with anhydrous ethanol to volume in a 10ml volumetric flask. Accurately weigh the naphthalene internal standard 513.55 mg was made up to a 50 ml volumetric flask with absolute ethanol. The above reference solution was accurately weighed into 0.2 ml, 0.4 ml, 0.6 ml, 0.8 ml, 1.0 ml, 2.0 ml, and 1 ml of the above naphthalene solution was precisely added to a 10 ml volumetric flask. Each concentration was injected once. Taking the menthol peak area as the ordinate and the menthol concentration (mg/ml as the abscissa, the norm curve is drawn, and the regression equation is calculated (n=6 is: Y=809.00X-1.02.r=0.9998.Y-peak area, X sample concentration (mg/ml

Under these conditions, the above results are indicated. The menthol concentration has a good linear relationship in the range of 0.101.30 mg/ml.

Calculated by the internal standard method, 2.4 precision experiments were taken at the same concentration of the test solution 1.0 μl and repeated injections 8 times. The RSD of 0.12% indicates that the precision of this method is good.

The concentration of 10.27 mg/ml of the internal standard naphthalene was separately added to prepare and measure the test solution according to the content determination method. The 2.5 repeatability experiment took 2.5 g of the same batch of the test sample. Calculated by the internal standard method, the RSD of 0.49% indicates that the method is reproducible.

The samples were injected at room temperature after 012361224 h, and the 2.6 stability test was taken at the same concentration. The average value of the 7 measurements was 0.55 mg/ml and the RSD was 0.49%. The results indicated that the test solution had good stability within 24 hours.

Add 1ml of the internal standard concentration of 10.13mg/ml and a certain amount of menthol reference solution, respectively. 2.7 Recovery rate test Take the same batch of known content of 2.5g6 parts. The preparation and measurement of the test solution were carried out according to the content determination method, and the results indicated that the recovery rate of the method met the requirements.

The method is highly sensitive, as evidenced by the above methodological findings. The precision, reproducibility and recovery coefficient of variation are all below 3%, which meets the requirements of the “Quality Specification” in the Technical Requirements for New Drug Research of Traditional Chinese Medicine.

3 Discussion

Three system conditions were selected: 1 detector with FID column temperature of 150 °C; injector temperature of 230 °C; detector temperature of 230 °C. The initial temperature of the 2 column temperature is 120 ° C, and the selection of the 3.1 system conditions is checked by reference. Adhere to 2min first to increase the temperature to 2 °C per minute to 140 ° C, adhere to 2min at 10 ° C per minute heating rate to 190 ° C, adhere to 10min split ratio for the 2013 inlet temperature of 250 ° C, detector temperature of 250 °C, the split ratio is 251 column temperature is 60 ° C, adhere to 5min at a temperature increase rate of 5 ° C per minute to 100 ° C, adhere to 2 min

Therefore, the system was used as the systemic condition for the determination of menthol content in swollen and painful aerosols. System (12 measurements of menthol peaks could not achieve baseline separation; system (3 determination of menthol peaks and adjacent peaks reached baseline separation and resolution) More than 1.5 separation effect is good.

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