Alpinia galanga Granule Preparation Process and Quality Control_111

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Alpinia galanga Granule Preparation Process and Quality Control_111

    Alpinia galanga Granule Preparation Process and Quality Control

     Authors: YE Juan, GAO Wen-Yuan, SUN Li Ya, Liu

    Xinqiao, Tie-Jun Zhang, Hai-Xia Chen, Wang Shujun

     Abstract Objective To determine the best Alpinia galanga

    granules preparation process, the establishment of Alpinia granules in eucalyptol method for the determination. Methods steam distillation Alpinia galanga medicinal herbs in the volatile oil, design L9 (34) orthogonal experiment to determine the optimum inclusion volatile oil process, the water extract of dried concentrated formula is made with the inclusion particles, using gas chromatography , FID detector determination of granules in the content of eucalyptol. Results will be 10 times the amount of medicinal water

    extracted 5 h, to collect extracts and volatile oils. Optimum inclusion volatile oil process: volatile oil and β-

    cyclodextrin ratio of 1:9, inclusion temperature is 45 ?,

    inclusion time was 1 h. Determination of the regression equation y = 2 635 4 x - 0.040 4, r = 0.999 8, average

    recovery was 100.72%, RSD of 2.58% (n = 5). Conclusion Alpinia granules preparation process is stable and feasible evaluation index a reliable and reasonable.

     Key words Alpinia granules; eucalyptol; volatile oil; gas


     Abstract: ObjectiveTo optimize the preparation process of Alpinia officiarum formula granules and establish a determination method of eucalyptol in the formula granules. MethodsThe volatile oil was extracted with steam

    distillation method and included with β cyclodextrin to

    avoid its volatilization. The granule was prepared by mixing the water extracts, volatile oil and starch. The content of eucalyptol in the granule was determined with the GC method.ResultsThe optimum extraction condition was as follows: the crude drug was extracted with 10 times amount of water for 5 hours to collect the volatile oil. The optimal inclusion condition selected by the L9 (34) orthogonal design was as follows, the ratio of volatile oil to β cyclodextrin was

    1: 9 (ml / g), the inclusion time was 1h and the temperature of the inclusion was 45 ?. The regression equation was y = 2 6 354 x 0.040 4, r = 0.999 8. The average recovery was 100.72% and RSD was 2.58%. ConclusionThe preparation process

    of Alpinia officiarum formula granules is stable and feasible. The GC method for quality control is accurate and suitable.

     Key words: Alpinia officiarum; Formula granules; Eucalyptol; Volatile oil; GC

     Galangal is a plant Zingiberaceae Alpinia Alpinia Alpinia

    officiarum Hance dry roots, the main produced in Fujian, Taiwan, Guangdong, Guangxi, Hainan, Yunnan and other places, with a warm stomach cold-dispelling, digestion analgesic

    efficacy, clinical commonly used in the treatment of Zhongwan

    abdominal Leng Tong, Wei Han vomiting, belching Tunsuan other diseases [1]. Modern pharmacological studies have shown that Alpinia galanga has a strong analgesic antiemetic [2], anti-

    ulcer, gallbladder, anti-diarrhea [3], antibacterial [4],

    anti-oxidation [5], anticancer [6] and so on.

     Alpinia Galangal Pieces formula particles by the extraction, concentration, drying and granulation processes such as traditional Chinese medicine made from a single-flavor

    granules. Pieces traditional Alpinia changed granules, can

effectively remove the plant fiber and other non-active

    ingredients, to increase stability, easy to store, easy to take. Granule its production automation, production conditions, constant, small man-made factors are widely used

    in clinical advantages. Coptis formula, such as particles, regardless of whether the same lot number, its berberine content are within the scope of the requirements in the determination of [7]. At present, about Alpinia galanga granules and determination of the preparation process have not been reported in this paper using gas chromatography control of particles in the cineole content. Are reported below.

     An instrument and reagent

     Agilent 6820 gas chromatograph (Agilent, USA); KQ218 ultrasonic cleaner Kunshan Ultrasonic Instrument Co., Ltd.; DZG 401 electric vacuum drying oven, Tianjin Tianyu instrumentation laboratory; Sartorius BS210S Electronic Balance Tianjin Ott Sainz Instrument Co., Ltd..

     Alpinia Pieces (Pieces by Tianjin Traditional Chinese

    Medicine Factory to provide), in line with "Chinese Pharmacopoeia" in 2005 edition of requirements; eucalyptol reference substance (Lot No. 110748 200507) purchased in

    China pharmaceutical and biological products. N-hexane, for

    chromatography pure cyclohexanone, ethanol, β

    cyclodextrin, starch, and other reagents were of analytical grade.

     2 Methods and Results

     2.1 Alpinia granules volatile oil extraction process to take Galangal 200 g, plus 10 times the amount of water extraction, measuring equipment used to collect volatile oil (light method) volatile oil, obtained at intervals of 1 h the amount of volatile oil volume, examining the rate of extraction time and out of the oil the relationship between the results in Table 1. From Table 1 we can see, the former 5 h out of the oil has reached 95.1% of the total. Therefore,

    extraction time of 5 h. Extraction time of the study in Table 1 (omitted)

     2.2 The volatile oil from Alpinia galanga β

    cyclodextrin inclusion

     2.2.1 Volatile oil inclusion process orthogonal experimental design pre-test results showed that the volatile oil and β cyclodextrin ratio (A), inclusion temperatures (B), inclusion time (C) that affect the outcome of the major

    factors Inclusion . On this basis, the design L9 (34) orthogonal to inclusion of the production rate and volatile oil inclusion rate as an index of the inclusion process parameters to inspect the level of the design factors in Table 2. Table 2 factors, level (abbreviated)

     2.2.2 Inclusion of volatile oil yield of investigation that take a certain amount of β cyclodextrin, according to

    the level of each factor orthogonal experiment with the order to join a certain amount of distilled water, heating allows the dissolved solution made of 2% at constant temperature magnetic agitator on the mixing to the required temperature, slowly dropping volatile oil ethanol solution, while stirring to the prescribed time plus side, put cold, home refrigerator for 24 h, leaching, following with 10 ml of petroleum ether

    (30 ~ 60 ?) washing , 40 ? drying 3 h, pulverization was

    inclusion, computing inclusion yield. The results in Table 3.

     Analysis of variance we can see from Table 4, volatile oil and β cyclodextrin ratio on inclusion yield

    significant factors, while the inclusion of temperature and time on the inclusion yield inclusion complexes have no significant effect.

     2.2.3 Volatile oil inclusion rate of the study under different conditions in order to study the pros and cons

    effects of inclusion in order to volatile oil inclusion rate as an indicator to analyze inclusion in the product contains volatile oil.

     Volatile oil inclusion rate = (V1 V2) / V × 100%; V1-

    recovery obtained from the inclusion complex of volatile oil

    (ml); V2-blank recovery experiment, the amount of the loss of volatile oil (ml); V-volatile oil investment Feeding Capacity (in this experiment is 1 ml).

     By analysis of variance in Table 4, we can see volatile oil and β ratio of cyclodextrin inclusion volatile oil from affecting the rate of significant factors, inclusion of temperature and time of inclusion volatile oil inclusion rate had no significant impact.

     Table 3 orthogonal L9 (34) program and data-processing%

     Table 4 Analysis of variance

     By the inclusion of the production rate and the rate of inclusion volatile oil analysis of two indicators can be seen, set the appropriate volatile oil and β cyclodextrin

    inclusion ratio is an important factor in product quality, pros and cons. According to visual analysis of the rate of inclusion can be seen well above the A2 and A3 mean A1, according to the rate of inclusion complex visual analysis of

    collected can be seen above the A3 and A2 means A1, comprehensive consideration, select the volatile oil and β

    cyclodextrin ratio of 1 : 9 most appropriate. Inclusion of temperature and inclusion time were non-significant factors,

    combined with visual analysis and cost options to B2C1. Therefore, the optimum inclusion process is A3B2C1.

     To verify the optimal process, repeated three times experiments, to be an average inclusion rate of 89.9%, with an average volatile oil inclusion rate was 88.8%, to certify that

    the inclusion process and reliable.

     2.3 Preparation of granules Alpinia galanga Alpinia granules in order after the optimization process, that is to take Galangal Pieces 500 g, plus 10 times the amount of water, micro-boiling extracts 5 h, while collecting extract and volatile oil. On the volatile oil inclusion process in accordance with the best package together, drying, pulverization, spare. Decompression of the extract was dried concentrated extract, vacuum drying, the dry extract and

    starch, the ratio of the mass ratio of 1:1 by adding auxiliary materials, mixing, add 75% of the amount of ethanol made from soft materials, soft materials over 14 sieve made of particles, 60 ? under vacuum drying 24 h. In accordance with

    the Central Plains and some herbs and then adding the proportion of volatile oil inclusion, mixing, or may Alpinia granules.

     Alpinia galanga granules 2.4 Qualitative Identification of

     2.4.1 Preparation for the test product solution to take

    Galangal granules of about 0.5 g, precision, said determined set of volatile oil extractor in water 200 ml, and the volatile oil extraction in the liquid inside the water, adding about 2 ml n-hexane extract 2 h get oil hexane constant volume to 5 ml, were tested product solutions.

     2.4.2 Preparation of the solution to take control medicine Galangal control medicines 5g, according to 2.5.4 under "for test preparation materials solution" approach, in contrast with the legal system, medicine solution. Reposted

    elsewhere in the paper for free download http://

     2.4.3 Preparation of negative control solution obtained in accordance with the proportion of prescriptions starch granules, β cyclodextrin and the water extracts of

    medicinal extract, according to test products for the preparation method of solution preparation, as a negative

    control solution.

     2.4.4 Identification of thin-layer chromatography in accordance with thin-layer chromatography (Appendix ? B)

    test, drawing negative reference substance solution, volatile oil, the above test items for the medicinal solution and control solution of 10 μl, respectively, points on the same silica gel G thin-layer board to toluene ethyl acetate

    (19:1) as the agent, started out, dried, sprayed with 5%

    vanillin sulfuric acid solution, heated at 105 ? to spot

    color definition. Test products for chromatography, chromatography with the corresponding control medicines may position, significantly the same color spots.

     Alpinia 2.5 Determination of Granule

     2.5.1 Gas chromatography conditions

     Column: HP 5 fused silica capillary (30 m × 0.32 mm,

    0.25 μm); temperature-programmed conditions: initial temperature of 50 ?, maintained 1 min, to 10 ? * min up to

    180 ?, and then to 20 ? * min up to 210 ?, maintained 1

    min; carrier gas N2; inlet temperature of 220 ?, FID detector

    temperature 250 ?, sample 1.4 μl.

     2.5.2 Preparation of reference substance solution

     Precision that will eucalyptol reference substance, with n-hexane dissolved, made of 14.096 mg / ml solution.

     2.5.3 Preparation of internal standard solution

     Precision that will cyclohexanone with n-hexane

    dissolved, made of 15.654 mg / ml solution.

     2.5.4 Preparation for the test product solution

     Alpinia granules take about 0.5 g, precision, said determined set of volatile oil extractor in water 200 ml, and the volatile oil extraction in the liquid inside the water, adding about 2 ml n-hexane extract 2 h, set in the oil-hexane

    solution flask, the precise internal standard solution, 1.10 ml, constant volume to 10 ml, shake, as a solution for the test items.

     2.5.5 linear relationship between the study

     Reference substance solution were collected from 100, 140, 180, 220, 260 μl, internal standard solution of 150 μl,

    constant volume to 5 ml, for gas measurement. To eucalyptol volume abscissa to eucalyptol peak area / internal standard area of the vertical axis bee, drawing standard curve obtained standard curve equation was y = 2 6354x -0.040 4, r = 0.999 8.

     2.5.6 Experimental precision

     Take a linear relationship in the first five samples of a continuous sample injection 5 times, the measured RSD = 0.76% (n = 5). Correction factor averaged 0.828 0.

     2.5.7 Reproducibility experiment

     Precision said the same group of samples taken five copies, according to test products for the solution preparation methods to operate, continuous sampling, the measured RSD = 0.845%.

     2.5.8 Stability test

     Precision that take a sample, according to test products for the solution preparation methods in parallel operation, at

    intervals of 2 h into the sample, a continuous 8 h, the results of the measured RSD of 1.59%.

     2.5.9 The average recovery experiment

     To 2.5.4 for the test items under Preparation of Solution Preparation of 5 copies of Alpinia granules sample solution by adding a certain concentration of reference substance solution and the internal standard solution, fixed volume measured, the

    measured average recovery was 100.72% , RSD is 2.58% (n = 5). Table 5 The average recovery experiment (omitted)

     2.5.10 Determination of Alpinia granules were taken three batches of high precision, said Liang Jiang granules, according to the method under 2.5.4 Preparation of test items for the solution, were measured to calculate cineole content. The results in table 6. Table 6 Alpinia granules assay results (omitted)

     3 Discussion

     3.1 Decoction preparation compared with the traditional

    advantages of Alpinia galanga granules as the main active ingredients of volatile oil, volatile oil extraction, by the method of extraction, and traditional Chinese medicine decoction with water extracts taken orally, dispensing granule decoction as the reform of traditional Chinese medicine On the one hand a form of play to the advantages of modern science and technology, on the other hand we have to maintain consistency with the traditional decoction, it finished first mentioned aqueous solution of volatile oil concentration

    drying, granulation, and then in accordance with the proportion of herbs to add some Central Plains inclusion volatile oil, blending to achieve both water-soluble

    components and volatile oil purposes.

     3.2 The conditions of inclusion volatile oil volatile oil chosen to study the inclusion criteria, respectively inclusion

    rate and the inclusion yield of indicators on the best conditions are not consistent, but inconsistent with the conditions, taking into account a non-significant factors in

    various level, but also from an intuitive analysis, we can see little difference between them, it is mainly from the economic costs of non-significant factors affecting the level of choice.

     The experimental method is simple and feasible,

    reproducible, can be used as control product quality.


     [1] National Pharmacopoeia Committee, Chinese Pharmacopoeia [S]. Beijing: Chemical Industry Press, 2005:202.

     [2] Daitetsu shin, Kauru Kinoshita, Kiyotaka Koyama, et

    al. Antiemetic principles of Alpinia officiarum. Kunio T [J]. J Nat Prod, 2002,65:1 315.

     [3] Zhu Ziping, Chenguang Juan, Zhang Ming Fa, et al. Alpinia galanga temperature and pain in pharmacological studies [J]. Chinese herbal medicines, 1991, 14 (10): 37.

     [4] Gong Yu Jing, Anjou States, Yuhui, et al. 164 kinds of traditional Chinese medicine ethanol extracts of anti-

    fungal effect of [J]. Chinese herbal medicine, 2002,33 (1): 42.

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