Abstract: Borneol acetate is a colorless to pale yellow liquid or white crystalline solid, slightly soluble in water, soluble in ethanol, has a cool pine fragrance, and has camphor-like breath. Borneol acetate is naturally found in fir oil and some essential oils of pinaceae plants, usually in the form of L-body.
Objective To establish a method for determining the content of Borneol acetate in volatile oil of Valeriana officinalis. Methods Gas chromatography was used, naphthalene was used as internal standard, DB-17 capillary column, carrier gas was helium, and electron bombardment (EI) ion source detector. Results Under this chromatographic condition, Borneol acetate showed a good linear relationship within the injection volume of 0.1096 ～ 1.7536μg, r = 0.9996; the recovery rate of Borneol acetate was 101.33%, RSD = 1.79%. Conclusion This method can accurately determine the content of borneol acetate in volatile oil of Valeriana officinalis.
1 Instruments and reagents
QP5050A GC-MS (Japan Shimadzu Corporation); AB-N electronic analytical balance (Mettler-Toledo Instruments Shanghai Co., Ltd.); micro pipette (Dalong Medical Equipment Co., Ltd.).
Black water valerian samples (collected from Huma area, Daxing'anling, Heilongjiang Province, identified as authentic by Professor Du Xiaowei); borneol acetate reference substance (China National Institute for the Control of Pharmaceutical and Biological Products, batch number 110759-200303); naphthalene and methanol are chromatography pure.
2 Methods and results
2.1 Chromatographic conditions DB-17 quartz capillary column (30m × 0.25mm, 0.25μm); carrier gas is high purity helium; flow rate 20ml / min; pre-column pressure 63kPa; initial temperature 80 ℃ (maintain 2min), 3 ℃ / The rate of min rises to 150 ° C (maintained for 3min), then rises to 220 ° C (maintained for 25min) at a rate of 10 ° C / min; the temperature of the gasification chamber is 180 ° C; the electron bombardment (EI) ion source detector, the electron energy is 70eV, Acceleration voltage 0.8kPa; detector temperature 250 ℃; split ratio 20: 1; mass scanning range 50 ～ 500m / z; scanning speed 0.5s / dec.
2.2 Preparation of test solution
2.2.1 Preparation of reference substance solution Precisely weigh the appropriate amount of the reference substance of beborneol acetate, add methanol to make a solution of 2.1920 mg / ml.
2.2.2 Preparation of internal standard solution Precisely weigh the appropriate amount of naphthalene, add methanol to make a solution of 2.0077mg / ml.
2.2.3 Preparation of test solution Weigh the right amount of black water valerian herbs, extract the volatile oil according to the method of determination of volatile oil in Appendix XD of the 2005 edition of the Chinese Pharmacopoeia, and accurately absorb 0.1ml of black water valerian volatile oil in a 25ml volumetric flask , Add 5ml of internal standard solution, dilute with methanol to the mark, shake well.
2.3 Investigation of linear relationship Accurately absorb 0.1, 0.2, 0.4, 0.8, and 1.6 ml of the reference solution, put them in 2ml volumetric flasks respectively, add 0.4ml of internal standard solution, and dilute with methanol to the mark. Accurately draw 1μl and inject it into the gas chromatograph for measurement. The regression is based on the ratio of the injection volume of the reference substance and the peak area of ​​the reference substance / internal standard to obtain the standard curve: Y = 0.4065X-0.0011, r = 0.9996 (n = 5). The results showed that the injection amount of Borneol acetate in the range of 0.1096 ~ 1.7536μg had a good linear relationship.
2.4 Precision experiment The third point of the reference solution under the linear experiment was continuously injected 6 times, and the average value of the ratio of the reference substance and the internal standard peak area was calculated to be 1.1543, RSD = 0.69%.
2.5 Reproducibility experiment The same batch of samples was measured 5 times from the beginning of sampling, and the average content was 0.1382g / ml, RSD = 2.04%.
2.6 Stability experiment Accurately draw 1μl of the test solution, inject the sample, record the ratio of the sample and the internal standard peak area, measure every 1h, measure the average content of 0.1404g / ml 7 times within 6h, RSD = 0.91% .
2.7 Sample recovery rate experiment: accurately draw 5 samples of known content, add a certain amount of Borneol acetate to determine and calculate the sample recovery rate.
2.8 Sample determination Take 5 batches of samples of Valeriana officinalis in different harvesting periods, prepare 5 sample solutions in parallel according to the preparation of test solution, and inject 1 μl of each sample to determine the content of Borneol acetate.
3 conclusions
The method uses naphthalene as the internal standard, which is sensitive, accurate and reproducible. It can accurately determine the content of borneol acetate in the volatile oil of Valeriana officinalis.
It can be seen from the measurement results of the samples that the content of borneol acetate in the volatile oil of the samples is slightly different in different harvest periods, the fruit ripening period reaches the highest value, and the content in the wilt period has decreased. Therefore, if the content of borneol acetate is used as a quantitative index to evaluate the volatile oil of Valeriana officinalis, the harvest should be the best when it is ripe.
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