Amomum compound Volatile Oil Extraction Process Optimization Study
Authors: TANG Can, WU Shi Choi, Yun-Peng Li,
Zhang Yanyan, Zhao, Pu Qing Rong, Lan Cai
【Abstract】 Objective Optimization of Amomum compound
volatile oil extraction process. Methods bornyl acetate yield as an indicator, using gas chromatography, using orthogonal design optimization Amomum compound volatile oil extraction process conditions. The results out of Amomum preferred compound volatile oil extraction as follows: take Amomum villosum smashed, other herbs cut into Pieces, add water, soaked in 0.5 h, add water, 96 times the amount of herbs, using steam distillation 4 h. Conclusion The extraction of volatile oils extracted the active ingredient compound Amomum
bornyl acetate yield high and stable, indicating that the process is reasonably practicable.
Key words Amomum compound volatile oil; bornyl acetate; gas chromatography; Extraction Process
Abstract: ObjectiveTo optimize the extracting process of
volatile oil from Amomum villosum etc.MethodsBy the orthogonal design and gas chromatography, taking the rate of Bornyl Acetate as the index, we optimized the extracting process conditions of volatile oil from Amomum villosum etc.ResultsThe
optimum extracting process conditions of volatile oil from
Amomum villosum etc.were that Amomum villosum was pounded to pieces, water was 96 times the weight of herbs, soaking time was half an hour and extracting time was 4
hours.ConclusionExperiment results make it clear that because the rate of bornyl acetate in volatile oil from Amomum villosum etc.by the optimum extracting process is high and stable, the extracting process of volatile oil from Amomum villosum etc. is reasonable and feasible.
Key words: Volatile oil from Amomum villosum etc.; Bornyl acetate; Gas chromatography; Extracting process
For Zingiberaceae Amomum Amomum villosum, green shell sand, dry sand of Hainan ripe fruit, with dampness qi, warm the vomiting diarrhea, the efficacy of tocolysis, mainly for the wet evil trapped spleen, the spleen and stomach qi stagnation, spleen and stomach Deficiency Pernicious vomiting and diarrhea as well as the stagnation of qi resistance, fetal movement disturbed embolism. Main-containing volatile oil, oil
One of the main active ingredient bornyl acetate (Bornyl acetate). As noted in reported in the literature, at present villosum and their proprietary Chinese medicine is based on the quality of essential oil yield to control. But the
volatile oil as the mixture of both composition and nature of the instability, as a quantitative standard is not quite perfect. Bornyl acetate and the structure is clear, high content, pharmacological experiments confirmed that bornyl acetate with Amomum attending closely related to the
effectiveness of the active ingredients. Bornyl acetate as a quantitative standard of Amomum villosum and their proprietary Chinese medicines are better than the volatile oil, can better control the quality of Amomum herbs and proprietary Chinese
medicines . Therefore, using gas chromatography with bornyl acetate yield as an index, optimization Amomum compound volatile oil extraction process has an important significance of quality control.
An apparatus and materials
GX 300A of nitrogen, hydrogen and air, one gas
generator (Beijing Zhongxing Technology Development Co., Ltd.), GC112A gas chromatograph (Shanghai Analysis Instrument Factory), double-ring brand of electronic analytical balance
(Shanghai Balance Instrument Factory), TG 328A analytical
balance (Shanghai Analysis Instrument Factory), 1 000,2 000 ml measuring equipment volatile oil (light oil), 20 μl micro-
pipette, 10 ml flask, 1 μl, 10 μl micro-syringe; Amomum
medicines purchased from Luzhou Glory pharmaceutical
companies, large white signs pharmacies, identified as Yang Chun sand. Ethyl acetate (AR), distilled water (homemade), bornyl acetate chemical reference substance (for determination by, 759 200102,0.2 ml) (Chinese medicines and biological
2 Methods and Results
2.1 GC analysis conditions  Column: 102 White silanized carriers (60 ~ 80 mesh), stationary phase 5% SE
30 (3 mm × 2 m, stainless steel column); column temperature: programmed temperature 80 ~ 140 ? (15 ? / min), 140 ~ 200 ?
(40 ? / min); carrier gas: N2 flow rate 30 ml / min; H2 flow rate of 20 ml / min; air flow rate of 200 ml / min, initial time, heating time, end times are 5 min, detector: FID; instrument: GC112A GC, GX 300A air, nitrogen and hydrogen
gas one machine.
2.2 The content of volatile oil from Amomum villosum and composition analysis of medicinal herbs such as more inclusive of volatile oil, which reached about 3.0% of Amomum villosum over oil, one of the most important component - the content of
bornyl acetate accounted for 25% to 30% so, we can see bornyl acetate as the main active ingredient Amomum villosum, one of the largest of its weight factor, and heat stability of bornyl acetate. It is extracted by steam distillation bornyl acetate
active ingredients of the method has sufficient theoretical
basis for the [3,4].
2.3 Process Optimization of Amomum such as medicinal herbs by steam distillation of volatile oil, bornyl acetate yield as an indicator to inspect steam distillation of the
best process conditions. Accurately take Amomum villosum and other medicinal herbs, said, according to L9 (34) orthogonal table, a total of nine copies of experiment, see Table 1 ~ 2.
Table 1 examine the factors level (abbreviated)
2.3.1 Preparation of volatile oil from Amomum medicinal herbs such as orthogonal solution, according to the above arrangements, steam distillation, collecting volatile oil, readings (ml), the nature of the use of oil-water separator,
oil in the water in the next, using 20 μl micro-pipette
device extraction of volatile oil, volatile oil dissolved in ethyl acetate and is scheduled to be tolerated by the 10 ml flask, namely, medicine and other essential oil may Amomum bornyl acetate solution; with ethyl acetate solvent as a blank control, to lack of Amomum villosum the other two drugs with the legal system, ethyl acetate solution as a negative control, storage and backup.
2.3.2 bornyl acetate standard curve drawing precision Weigh bornyl acetate Chemical Reference 0.192 7 g, dissolved in ethyl acetate and is scheduled to be tolerated by the 10 ml flask, the preparation of bornyl acetate reference substance solution concentration of 19.27 mg / ml, in 2.1 under the conditions of GC analysis of the determination of bornyl acetate Chemical Reference Points area of A and its quality of M showed a good linear relationship: A = 6 070.157 2 51 976.565 4 M , r = 0.999 0 (n = 6), linear range: 0.038 54 ~ 19.27 μg. Reposted elsewhere in the paper for free download
Table 2 Amomum medicinal herbs such as essential oil extracted orthogonal design experiments (omitted)
2.3.3 Repeatability experiments and optimization process for review in accordance with preferred out of Amomum
experimental medicine and other essential oil extraction process A2B3C1D1 cast material, extracted six times volatile oil, were determined oil content of bornyl acetate, bornyl acetate yield results for the medicine amount of (0.727 6 ?
0.018 15)%, n = 6, RSD = 2.49%, shows A2B3C1D1 process can be repeated and will be a good bornyl acetate extract the highest levels.
2.3.4 Experiment and the stability of precision experiments, bornyl acetate reference substance solution,
19.27 μg / μl, into the 0.5μl / times, from 2005 12
23 pm 21:40 pm 14:00 every 36 min Determination of 1 times, measured 12 consecutive times, the integral area of the experimental precision and stability of the experimental RSD
(%). One stability test RSD = 3.31%, that bornyl acetate within 6 h in the determination of concentration is stable; precision of RSD = 2.06%, showed good precision test equipment.
2.3.5 The average recovery experiments have been determined
to take bornyl acetate content of Amomum villosum, adding bornyl acetate reference substance, with extraction by volatile oil from Amomum bornyl acetate in the assay method. The results in Table 3.
Table 3 Amomum volatile oil, bornyl acetate recoveries
2.3.6 Determination of sample taking herbs such as essential oil Amomum bornyl acetate solution ? ~ ? samples,
respectively, injection 1 μl, at 2.1 GC analytical conditions were measured using the standard curve method content, the
results shown in Table 2, preferred out the optimum for A2B3C1D1. After review of experiments to prove A2B3C1D1 best. About Amomum villosum smashed, other herbs cut into Pieces, plus the amount of water, herbs 96 times, soaking 0.5 h, steam
distillation extract 4 h, Amomum medicinal herbs such as
volatile oil yield of bornyl acetate (0.727 6 ? 0.018 2)%, n
= 6, RSD = 2.49%.
In the experiment has compared the 5% SE 30,2% OV
17 two kinds of GC column packing, according to Amomum volatile oil bornyl acetate, camphor of the chromatographic behavior into account, with 5% SE-30 compared withWell. And
carried out isothermal experiment compared with the programmed temperature and found that the preferred temperature-
programmed chromatograms. And temperature-programmed to a
first-order and second-order temperature tests, found that
second-order temperature-programmed (80 ~ 140 ?, 15 ? / min,
a first-order; 140 ~ 200 ?, 40 ? / min, second-order) were a
very good color spectrum. Figure 1. Bornyl acetate camphor peak and impurity peaks separation, peak symmetry, number of theoretical plates are best. Ethyl acetate blank control without interference, lack of Amomum the other two drugs ethyl acetate solution of non-interference with the negative control with satisfactory results.
a Chemical Reference b samples c blank reference
Figure 1 Gas chromatogram (omitted)
Unilateral right Amomum villosum extract the volatile oils and three kinds of Chinese herbal compound extracts such as essential oil. The results showed that compared levels of unilateral extraction and compound derived from extraction of
volatile oil content of bornyl acetate big difference. Unilateral determination of volatile oil extracted by fewer,
but higher content of bornyl acetate; compound of volatile oil extracted more, but bornyl acetate at low levels. The Department of compound may be extracted when the three kinds of volatile oil emulsion with each other to produce interference, resulting in bornyl acetate in the column is more difficult to separate (as measured 8 h compound extracted bornyl acetate content of 4 h rather than the extract is low,
may be the Department of The longer the compound extraction, volatile oil emulsified with each other more thorough separation of the more difficult), or three kinds of volatile oil in the gasification chamber is about 200 ? temperature,
chemical changes caused bornyl acetate content decreased, and its mechanism needs further study.
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