3 Determination of butter in the borneol
【Abstract】 Objective To establish a quality control method of butter 3. Method of gas chromatography. PEG 20M as the
stationary phase, coating concentration of 10%, column length
3 m, were detected by FID, carrier gas nitrogen; Column temperature: 150 ?. Results 1.0 ~ 5.0 mg / ml range a good linear relationship, with an average recovery of 100.7%, RSD 1.5%. Conclusion The method is simple and efficient, accurate and reliable, and can be used for quality control of butter 3.
Key words three butter; borneol; gas chromatography
Abstract: ObjectiveTo establish a standard of controling the quality of Sanhuang oil.MethodsThe determination was carried out by GC.Chromatographic conditions were 10% PEG
20M as a stationary phase.The length of the column was 3 m. Flame ionization detector. The carrier gas was Nitrogen.The column temperature was 150 ?. ResultsThe linear relationship
was good in the range of 1.0 ~ 5.0 mg / ml. The average
recovery was 100.7%, and the RSD was 1.5%. ConclusionThis method is simple, convenient, rapid, accurate and reliable.This method can be used to control the quality of Sanhuang Oil.
Key words: Sanhuang Oil; Camphol Borneolun Syntheticum; GC
Third, home-made butter is the northern Jiangsu People's Hospital of Chinese medicine preparations, containing Coptis chinensis, Phellodendron, Huang Qin, borneol and other ingredients. Commonly used in clinical surgical wound can be an alternative medication for burns, skin laceration,
superficial soft tissue defect, wound infection, abscess drainage and treatment of pressure sores . , One of three active ingredients in butter borneol, Chinese medicine that its Weixin, bitter, sexually cold, in the final heart, spleen,
lung, there is resuscitation Xingshen, heat and pain relief, tissue regeneration achievements. "Materia Medica Spreads out Righteousness" that borneol "lone is potential weak Satsukai is meritorious." Modern medical research shows that borneol
has antibacterial, anti-inflammatory and analgesic efficacy
. 3 pharmacological effects of butter and similar pharmacological effects of borneol. As a result, we will be the content of borneol as an indicator as to control the quality of butter 3.
An instrument and reagent
GC 122 gas chromatograph (Shanghai Precision
Scientific Instrument Co., Ltd. Manufacturing); FID detector; N2000 chromatography data workstation (Zhejiang University Intelligent Information Engineering Research Institute); balance (Shanghai Precision Balance).
1.2 Drugs and reagents borneol reference substance (Chinese pharmaceutical products provided by the test); salicylic acid methyl ester (Shanghai Ling Feng Chemical Reagent Co., Ltd.), ethyl acetate (Shanghai Chemical Reagent Co., Ltd.) for AR.
1.3 Chromatographic conditions Column: PEG 20M as the
stationary phase, coating concentration of 10%, column length 3 m, were detected by FID; carrier gas: nitrogen 0.09 MPa
Column temperature: 150 ?; Gasification chamber temperature: 200 ?; detector FID: temperature of 200 ?, hydrogen 0.09
MPa, air 0.15 MPa.
Two methods [3 ~ 6] and results
2.1 Preparation of the tested products
2.1.1 Preparation of internal standard solution precision, said water to Yang methyl ester 250 mg in 50 ml Liang Ping, vinegar acid ethyl ester dissolved and diluted to the scale, shake, formulated into a concentration of 5 mg / ml solution.
2.1.2 Preparation of reference substance solution precision Weigh 250 mg of borneol reference substance in 25 ml Liang Ping, the vinegar acid ethyl ester dissolved and diluted to the scale, shake, that is, too.
2.1.3 Preparation for the test product solutions that take the butter at about 2.0 g in three 10 ml Liang Ping, the vinegar acid ethyl ester dissolved and diluted to the scale,
shake, filter, take added filtrate that was.
2.1.4 Preparation of blank samples according to the proportion of prescriptions will Coptis, Phellodendron, Scutellaria baicalensis soaked with vegetable oil 1 week, slow fire heated to orange, to residue, filtration. After the
heating and melting beeswax filtration, pour the vegetable oil, stirring evenly, that is, too.
2.2 The system suitability experiment were collected from a blank solution, reference substance solution and test products for the solution of 1 μl into the gas
chromatography, chromatogram shown in Figure 1 ~ 3. Under these conditions, with satisfactory results.
The linear range of 2.3 to take precise amount of borneol reference substance solution 1.0,2.0,3.0,4.0,5.0 ml to 10 ml,
respectively Liang Ping, add the internal standard solution 1 ml, combined with ethyl acetate to scale, shake. Accurately draw 1 μl injection, operating under the above
chromatographic conditions. With the concentration of borneol (c) as the abscissa, borneol and iso-borneol two peaks of the
peak area and with the internal standard peak area ratio (S) for the vertical axis for the standard curve regression equation was S = 2.262 3C 0.032 8, the correlation coefficient r = 0.999 5, that is 1.0 ~ 5.0 mg / ml within the framework of a linear relationship was good.
2.4 The precision experiment to take borneol reference substance solution, repeat sample 5 times. The results in Table 1. Table 1 borneol precision experiment (omitted)
2.5 repeated experiment reposted elsewhere in the paper for free download http://
Precision Weigh the same batches of three copies in 10 ml butter 5 in Liang Ping, each about 2.0 g, internal standard solution 1 ml, was diluted to scale combined with ethyl
acetate, shake, filter, filtrate continued to take a μl
sample. Calculation of the sample content of borneol. As shown in Table 2. Table 2 borneol repetitive experiments (omitted)
2.6 The average recovery
Experiment 9 blank samples were taken, respectively, by
adding the sample precision reference substance solution, according to the sample measurement method. The results in Table 3. Table 3 Borneol recovery assay (abbreviated)
2.7 Sample Measurement
Precision Weigh about 2.0 g of the product in 10 ml Liang Ping, add the internal standard solution 1 ml, combined with ethyl acetate to scale, shake, filter, take the filtrate added
1 μl sample to calculate concentration. Determination of three batches. The results in Table 4. Table 4 Determination of borneol samples (omitted)
3.1 in the pre-experiment, we use the content of
berberine as an indicator to control the quality of butter 3. In the extraction of berberine, we used a variety of programs, first used ether defatted, and then methanol extraction, thin layer chromatography, the sample does not appear with the corresponding spots of berberine. Analysis of the oil phase may be due to too much, not able to berberine isolated. So we use diatomaceous earth to the oil mixing Oil exhaustion, coupled with methanol, dissolved, reflux 15 min, will return to liquid filtration, liquid filters for thin-layer would be
launched, the same sample does not appear with the corresponding spots of berberine. So we switched to the oil to make oil-absorbing mixing diatomaceous earth, add acetonitrile -0.1% phosphoric acid, plus 0.1 g of sodium lauryl ultrasonic
oscillation 15 min, filter, filtrate obtained, TLC launched, samples have not yet seen with the corresponding spots Berberine. Analyze the reasons may be Berberine butter in three relatively low solubility, can not serve as determination of indicators. Through the literature review and found that three of the pharmacological effects of butter and similar pharmacological effects of borneol, so we will be the content of borneol as an indicator to control the quality of butter 3.
3.2 Column chromatographic separation is a key part, the author, taking into account the chemical composition of one of borneol borneol, for the larger polar compounds, so use 10% PEG-20M as a column.
3.3 3 in Borneol butter extracted by ethyl acetate, accessories, and other interference with fewer components,
extraction rate, can be used for gas chromatography. The method is simple and reliable, a good separation, high recovery rate can be used as indicators of the quality control of this product.
3.4 Natural borneol by Long of the brain and Isoborneol composition, so as to determine the content of the natural borneol and iso-borneol borneol the sum calculated. Borneol in the standard curve drawn to borneol and iso-borneol Peaks area
of the two, and as a whole, except within a standard substance peak area as the vertical axis, thus reducing sampling error.
3.5 Determination by borneol, making the content of borneol prescription under control, which can guarantee the efficacy of agents.
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