Compound consumption by the pain capsule Cyperus rotundus, cinnamon essential oil extraction and Inclusion Process
【Abstract】 Objective To study the Cyperus rotundus and cinnamon essential oil extraction and β cyclodextrin the
optimum. Methods orthogonal to study water multiples, medicines soaking time and distillation time on the impact of volatile oil extraction; to volatile oil inclusion rate and the inclusion of the yield of comprehensive evaluation, using orthogonal experimental design optimization β cyclodextrin
All process conditions. The results of the optimal extraction conditions, medicinal herbs, soaked 12 h, plus 10 times the amount of water, distillation 8 h; optimum inclusion conditions, volatile oil and β CD of the feed ratio of
1:6, inclusion temperature at room temperature, pack combined time of 3 h. Conclusion selected extraction and inclusion conditions, reached the highest yield of volatile oil revenues and inclusion high yield, and the purpose of inclusion with
Key words compound volatile oil consumption through the pain capsule orthogonal β CD
Study on the Extraction of Volatile Oil of Xiangfu and Rougui and its Inclusive Compound in Fufangxiaojingtong Capsules
Abstract: ObjectiveTo study the optimum extraction
process of volatile oil of Xiangfu and Rougui and its inclusive compound by Betacyclodextrin (β CD) in
Fufangxiaojingtong (FFXJT) Capsules. MethodsThe effects of water content, soaked and distilled time on extraction of
volatile oil were investigated and the technological process of inclusion compound by β CD were evaluated by orthogonal
design. ResultsThe optimum extracted conditions were to add ten times amount of water into the mixture of crude drugs, to soak for 12 hours and to distill 8 hours. The optimum conditions of preparation of inclusive compound were the proportion of 1:6 (volatile oil and β CD), 3 hours of
inclusion and ordinary temperature. ConclusionThe above technological process is the most rational.
Key words: Fufangxiaojingtong Capsules; Volatile oil; Orthogonal design; βCD
Compound consumption dysmenorrhea Capsules Astragalus, peony root, cinnamon, Cyperus rotundus, etc. composed of nine Chinese herbal medicines. Clinical for the treatment of
dysmenorrhea with good results. One cinnamon cold-dispelling
pain, promoting blood circulation, containing volatile oil 1% ~ 2%, mainly composed of cinnamic aldehyde, a sedative and analgesic effects , is the main effect of this drug ingredient. Cyperus rotundus Qi Jieyu, menstruation pain, for liver Qi stagnation, amenorrhea, dysmenorrhea. Contained 1% of the volatile oil has estrogen-like activity, along with
sedative and hypnotic effects, inhibit uterine contraction and other activity, the main component α Cyperone prostate
biosynthesis inhibitors , so Cyperus rotundus volatile oil is also the main effect of this product ingredients. These volatile components in the production and storage easy to damage and oxidation in metamorphism, thereby reducing the
efficacy. To solve this problem, to be the first to use steam distillation method of extracting volatile oils contained in cinnamon and Cyperus rotundus, and then β cyclodextrin (β
CD) will be volatile oil inclusion. In this study, the
orthogonal experimental method optimizing the extraction of volatile oil and inclusion processes.
A materials and equipment
Cinnamon purchased in Shijiazhuang lerentang Pieces Factory (Origin: Fujian), Cyperus rotundus medicine company,
purchased in Shijiazhuang Shenwei Pieces Factory (Origin: Hebei). β cyclodextrin, (content "98%), Beijing pairs of rotating micro-media products factory; anhydrous ethanol, analytically pure, Tianjin Standard Technology Co., Ltd..
Electric mixers, Nanhui, Shanghai Telecommunications Equipment Factory; HH * S11 2-type constant temperature
water bath pan, Beijing Chang'an Scientific Instrument Factory; DZF 6050 vacuum oven, laboratory equipment Co., Ltd. Shanghai Jingyi Wang; SHB 111 Multi-purpose type of
recycled water vacuum pump, Zhengzhou Great Wall Industry and Trade Co., Ltd. Branch.
2 Methods and Results
2.1 Volatile Oil Extraction Process
2.1.1 Extraction of essential oil of compound eliminate
menstrual cramps capsule according to the proportion of prescriptions, saying that taking Cyperus rotundus 220 g, cinnamon 110 g of volatile oil extraction devices in the home, by adding the provisions of times the amount of water, soak a
certain time, according to "Chinese Pharmacopoeia" 2005 edition of the Department ? Appendix XD Determination of
volatile oil (steam distillation) the allotted time, read the volatile oil.
2.1.2 Optimization of volatile oil extraction process according to the pre-experimental results, the two drugs
contained in the volatile oil are heavy fuel oil can be co-
distillation. Affect the amount of volatile oil extraction main factors are: water multiplier (A), medicinal herbs soak time (B), and the distillation time (C). Pairs of each factor to determine three levels, with L9 (34) orthogonal to the amount of volatile oil extraction for the evaluation indicators, essential oil extraction process of optimization, factor levels in Table 1. Orthogonal experimental results in
Table 2. Table 1 Volatile oil extraction factor level table (slightly) Table 2 Volatile oil extraction and the results of orthogonal experiment table (abbreviated) Table 3 Volatile oil extraction analysis of variance (abbreviated)
Pairs of orthogonal experimental results analysis shows that the impact of volatile oil extraction time is an important factor in the extraction, followed by soaking time, both the experimental results have a significant effect, add
water, no significant effect. Affect the degree of C> B> A.
Optimum condition is A2B3C3, namely medicinal herbs soaked 12 h, plus 10 times the amount of water, distilled 8 h.
Take 4 copies of medicines in accordance with the extraction process was optimized to validate the results of
the extraction of volatile oil were 2.8,2.6, 2.6, 2.7 g, RSD = 3.58%. This process is stable. Reposted elsewhere in the paper for free download http://
2.2 The Process of inclusion volatile oil
2.2.1 volatile oil β CD inclusion complex
Preparation of saturated solution method , taking β CD
plus saturated aqueous solution made from distilled water, and placing 250 ml triangular flask, in the specified temperature, in a certain mixing speed, precision dropping a certain amount of volatile oil: ethanol (1:1) solution, stirring inclusion specified time, take out, home refrigerator (4 ?) to place 24
h, leaching, with a small amount of anhydrous ethanol wash three times, vacuum dried solids 60 ? to constant weight, was
2.2.2 Volatile oil inclusion Optimization of process conditions based on test results reported in the literature and pre-determined inclusion volatile oil of the main factors are: volatile oil β CD ratio of inclusion time,
inclusion temperatures; 3 for each factor in determining the level of , using L9 (34) orthogonal to the yield of volatile oil revenues and the inclusion rate for the evaluation of indicators for inclusion technology of optimization, the
weights were 0.4 and 0.6. Factors in Table 4. Orthogonal experimental results shown in Table 5, analysis of variance results in table 6. Table 4 Volatile Oil β CD inclusion
factor level table (a little) Table 5 Volatile Oil β CD
inclusion of the orthogonal experimental results (omitted)
Table 6 volatile oil β CD inclusion analysis of
Actual results of the orthogonal direct analysis and variance analysis shows that volatile oil β CD and the
inclusion of the proportion of time on the experimental results are very significant impact of inclusion temperature
had no significant effect, affecting the degree of A> B> C. Optimum inclusion process is A2B2C1, the volatile oil and β
CD of the feed ratio of 1:6, inclusion time was 3 h, inclusion temperature at room temperature. 3 copies of essential oil obtained by optimizing the best technology of a verification experiment, the results of inclusion volatile oil
from an average rate of 86.1%, 75.6% yield of inclusion complex, indicating that this process is stable.
2.3 β CD Identification of volatile oil inclusion
2.3.1 TLC 
Sample Preparation: Take volatile oil 0.15 g buy 100 ml
flask, add petroleum ether to the scale, as a test product for the solution of A (positive control); taking β CD
inclusion volatile oil finished 0.15 g, plus petroleum ether wash, filter Guo, petroleum ether filtrate added to the fixed volume 100 ml, as a solution for the test product B; taking β
CD inclusion volatile oil plus 95% ethanol was extracted 30 min, filtration, the filtrate constant volume of ethanol added to 100 ml, as a test items for the solution C; taking β
CD 1 g, plus 95% ethanol was extracted 30 min, filtration, the filtrate constant volume of ethanol added to 100 ml, as a solution for the test product D (negative control).
TLC: lessons of the above-mentioned four kinds of
solution, 5 μl, points in the same piece of silicon G CMC
Na thin, and with petroleum ether ethyl acetate (17:3)
as the agent, started out, dried spray dinitrophenylhydrazine test solution, view, test products for the solution in the A, C chromatography, in the corresponding position, substantially
the same color of the spots shows that, after inclusion mention made of the volatile oil components has not changed, The test items for the B, D (negative sample) chromatography in the absence of such spots, indicating β CD volatile
oil from the formation of inclusion complexes has been very good. The results shown in Figure 1.
2.3.2 Identification of UV spectra  basically the same sample preparation TLC. Using UV spectrophotometry, scanning range of 200 ~ 400 nm, to absorb the absorption peak position
of the curve to determine the formation of inclusion complexes, in the results shown in Figure 2 ~ 5. Figure 2
shows UV spectra of volatile oil, 284 min are characteristic absorption peaks. Figure 3 for inclusion re-distilled volatile
oil obtained UV spectrum, maintaining a characteristic absorption spectral features, indicating a result of volatile oil package and the ingredients do not change; Figure 4 UV spectrum for the inclusion, 284 min without the characteristic absorption peak Note the formation of inclusion complexes of molecular very good; Figure 5 for the β CD distillation of
the negative control.
By Cyperus rotundus and cinnamon essential oil extracted from the optimum study found that water increases the amount
of volatile oil extraction had no significant effects, while the extraction time and soaking time has a significant impact. This may be due to the root bark of Cyperus rotundus and cinnamon is a class medicine, require a long soak, the moisture can soak into the dense organization of plant cells, so that slipped out of the volatile oil with the water vapor.
By TLC and UV identification, we can see Cyperus rotundus, cinnamon essential oil inclusion complex of volatile oil no longer has the original and UV spectral characteristics of thin spots. Note the formation of inclusion complexes of molecular very good. Inclusion complex recovered by distillation of the volatile oil TLC and UV characteristics of the original volatile oil similar to prove that the process of
inclusion volatile oil preserve quality.
Compound consumption by the Central Plains pain capsule production process will be volatile oil spray before loading the capsule particles, volatile oil components poor stability, reduce the effect. After the process is made through the inclusion loaded capsules, so that the stability and efficacy of agents have increased.
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