Abstract: Naotong injection is a lysergic acid derivative, which has the vasodilator effect of α-receptor blockade and can strengthen the metabolism of brain cells, increase the use of blood oxygen and glucose, improve mental disorders, and promote the neurotransmitter dopamine Replacement, stimulate nerve conduction to improve mental and emotional abnormalities.
Objective To simultaneously determine the contents of isoborneol and borneol in borneol by gas chromatography. Methods Naphthalene was used as the internal standard, and the internal standard was added in advance. The elastic quartz capillary column DB-WAX (30m × 0.32mm, 0.25μm), FID detector, nitrogen was used as the carrier gas, and the column temperature was 110 ℃. Results Under the chromatographic conditions, isoborneol, borneol and internal standard naphthalene were all well separated, and the recovery of borneol was 96.58% (RSD = 1.01%). Conclusion The method is sensitive, accurate and reproducible, and can be used to control the quality of the preparation.
Naotong injection is a compound preparation composed of 8 Chinese herbs such as astragalus, gardenia, borneol, etc. It has the functions of cooling blood, promoting blood circulation, rejuvenating the brain and rejuvenating the brain. Clinically used for stroke coma and cerebral embolism caused by cerebral stasis. In this experiment, a gas chromatographic determination method of borneol in the preparation was established to control its quality [1 ~ 3].
1 Instruments and reagents
1.1 Instrument Agilent 6890N gas chromatograph, FID detector; elastic quartz capillary column DB-WAX (30m × 0.32mm, 0.25μm).
1.2 Reagent borneol reference substance (batch number 743-8902), purchased from China National Institute for the Control of Pharmaceutical and Biological Products.
2 Methods and results
2.1 Chromatographic conditions and system suitability experiment H2 flow rate is 30ml / min, air flow rate is 400ml / min; column temperature is 110 ℃; inlet temperature is 200 ℃, detector temperature is 200 ℃, split ratio is 12: 1.
Prepare a negative control sample of borneol raw materials according to the prescribed amount, and measure according to the above chromatographic conditions. The chromatograms of the test solution, the Borneol reference solution, and the negative control sample solution are compared. The results are in the text. The peak can reach baseline separation, and the chromatographic peak in the negative control solution does not interfere with the determination.
2.2 Determination of correction factor Take an appropriate amount of naphthalene, dissolve with ethanol, and dilute to a solution containing 2mg per ml, shake well as the internal standard solution. Another appropriate amount of borneol reference substance, dissolved in ethanol and diluted to a solution containing 1.5mg per ml, shake well, as a reference solution. Accurately draw 2ml of reference solution and 1ml of internal standard solution, mix well; take 1μl and inject it into the gas chromatograph to calculate the correction factor.
2.3 Preparation of the test product solution Precisely absorb 2ml of this product solution, precisely add 1ml of internal standard solution, mix well; take 1μl and inject it into the gas chromatograph, measure, calculate and get.
2.4 Sample solution stability experiment Take the test solution of the same batch number (060312), accurately draw 1μl, sample at a certain time interval, measure, and conduct peak area inspection. The total peak area of ​​isoborneol and borneol is 520.52 , RSD is 2.15%. The results show that the test solution is basically stable within 12h.
2.5 Precision experiment (repetitive experiment) Take 6 copies of Naotong injection of the same batch, and test the content in parallel according to the content determination method. The result is the content of borneol (total of isoborneol and borneol) is 1.52mg / ml.
2.6 Investigation of linear relationship Precisely weigh an appropriate amount of borneol reference substance, add ethanol to dissolve and make a solution containing 15mg per ml as a stock solution. Accurately measure 0.2, 0.4, 0.6, 1.0, 1.5, 2.0ml of the reference stock solution in a 10ml measuring flask, add the internal standard solution to the mark, and shake well. Accurately draw 2ml of each reference solution, add 1ml of internal standard solution precisely, and mix well; take 1μl and inject it into the gas chromatograph, determine the peak area according to the chromatographic conditions described in the text, with the concentration as the abscissa (X), the peak area of ​​the reference The ratio of the internal standard peak area is the ordinate (Y), draw a standard curve, and calculate the regression equation.
The linear equation is: Y = 0.6849X + 0.0083, r = 0.9998
The results showed that borneol (total borneol and borneol) had a good linear relationship in the range of 0.30 ~ 3.0mg · ml-1.
2.7 Recovery rate experiment Blank preparations (6 copies) were prepared according to the prescription, accurately weighed, and appropriate amounts of borneol reference substance were added at different ratios respectively. According to the above chromatographic conditions, the total recovery of isoborneol and borneol were calculated.
The above results indicate that this method has a good recovery rate.
2.8 Sample determination 3 batches of this product, measured according to the method described in the text, calculated the content of borneol is 1.52mg / ml (batch 060312), 1.56mg / ml (batch 060315), 1.48mg / ml (batch 060318) .
3 Discussion
Borneol raw materials in pharmaceutical preparations are usually synthetic products, and isoborneol is generated during the production process, which is analyzed by gas chromatography as two peaks. Therefore, when calculating the content, the sum of isoborneol and borneol peak should be taken. The raw materials from different sources have obvious differences, so the quality of the synthetic borneol should be controlled, and the product should be measured before feeding.
In the experiment, various parameters of the chromatographic conditions, such as temperature, were optimized. As a result, the chromatographic peaks of isoborneol and borneol peak reached a good separation at 115 ℃, the peak shape was good, and the number of theoretical plates was high.
This experimental method has high sensitivity, good specificity and reproducibility, easy operation, and can be used for the quality control of Naotong injection.
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