| Objective:Frankincense,cartesian frankincense tree for olive branch plants Boswellia carterii Birdw.and the same plant bao of frankincense tree Boswellia bhaurdajiana Birdw.bark out of the resin.There are only source,character,identification,content determination and impurities test,and among of content determination item only containing volatile oil content determination in the 2015 edition of China pharmacopoeia of frankincense medicinal quality standard,so that frankincense quality standard need to add and perfect.Rules of origin of frankincense in the pharmacopoeia only two kinds:Ethiopia and somalia,but through the literature and research the market survey,the circulation of many medicinal materials are made in domestic or other countries.With the existing different identification methods,there exists problems in different degrees such as large dosage of herbs,not enough objective and time-consuming.To solve above problems,our topic proposed two kinds of new technology.Using TG-DTA thermal analysis to quickly identify traditional Chinese medicine frankincense and the quality analysis;Using infrared spectroscopy to identificate authenticity of frankincense and achieve rapid determination of effective components content in frankincense,which used to evaluate the quality of frankincense.Exploring rapid,accurate and simple identification methods of frankincense medicinal materials quality evaluation is of great significance.Research and Method:Including sample collection,traditional identification of frankincense,quickly identify traditional Chinese medicine frankincense and quality analysis by using TG-DTA thermal analysis,qualitative and quantitative research by Infrared spectroscopy of frankincense.1 Sample Collection In Hebei amara Chinese herbal medicine market,Anhui bozhou herbs market,Beijing tongrentang,Shandong,Jilin,Gansu,Sichuan,Guizhou,Guangxi,Hangzhou,Ethiopia and other places,41 batch of frankincens samples have been collected,including 15 batches of frankincense,26 batch of frankincense.2 Traditional Identification According to the 2015 edition of China pharmacopoeia to identify frankincense collected by experiment,which determined the collected samples of frankincense cartesian frankincense tree for olive branch plants Boswellia carterii Birdw and the same plant of frankincense tree Boswellia bhaurdajiana Birdw.bark out of the resin or not.According to the literature method,using thin layer chromatography method,comparing with spots of the article 11-carbonyl acid-beta-acetyl frankincense and contrast medicinal herbs to identify frankincense.To draw UV scanning curve control intercomparison of the sample under the 200-400 nm wavelength ultraviolet wavelength scanning,and then identify the the authenticity of the sample.To determine 11-carbonyl-beta-acetyl frankincense acid content in frankincense by using high performance liquid chromatography.3 Quickly identify traditional Chinese medicine frankincense and quality analysis by using TG-DTA thermal analysis Inspection influence of three factors of temperature,heating rate,powder particle size on the TG-DTA thermal analysis experiments,and identify the authenticity of medicinal materials rapidly using TG-DTA feature maps;Using first order points and connection method to make thermogravimetric analysis and heat enthalpy calculation to quantitative analysis frankincense respectively.4 Qualitative and quantitative research by Infrared spectroscopy of frankincense Applying fourier transform attenuated total reflection infrared spectroscopy for qualitative detection of frankincense;Applying near infrared diffuse reflectance infrared spectroscopy and fourier transform attenuated quantitative calibration model for quantitative analysis of content of 11-carbonyl-beta-acetyl frankincense acid in frankincense.Result:1 Traditional Identification(1)Character Identification According to the 2015 edition of Chinese pharmacopoeia to character identify collected frankincense.The result showed that 36 groups of frankincense in 41 are official,which is the cartesian frankincense tree olive plants Boswellia carterii Birdw.and the same plant bao of frankincense tree Boswellia bhaurdajiana Birdw.bark out of the resin;5 batches are unofficial.Three batches are inferiority of quality.(2)Thin-layer Identification In TLC experiment,the spots of 2 batches of samples of goods at corresponding positions does not appear and spots of three batches of samples is not obvious.(3)UV Identification In UV identification experiment,the fitting between tultraviolet absorption curve of two batch of samples and ultraviolet absorption curve of contrast herbs is poor,which chromatographic peak of the second and third of three groups of samples disappear or not obvious.The second chromatographic peak of ultraviolet absorption curve of 3 batches of samplestransition is not smooth,where the third chromatographic peak almost not appear,and other batches to frankincense have no obvious difference between the ultraviolet spectrum.(4)High performance liquid chromatography method for determining the content of effective component The range of content of 11-carbonyl-beta-acetyl frankincense acid in frankincense measured by high-performance liquid chromatography is 0.07?0.07,of which 5 batch of sample did not reach reference content of 2.0%.The results identified by four traditional identification methods showed that the two batch of falsify and three batch of shoddy are consistent.2 Quickly identify traditional Chinese medicine frankincense and quality analysis by using TG-DTA thermal analysis This study determines the best experimental conditions of TG-DTA of frankincense:Temperature range 50-750?;The heating rate select 2?/min;Powder mesh choose 100 mesh;Under the condition,through the characteristic peak(T1 =447± 5?,T2=Z 549 ±5?,T3 = 350 ±5?),thermogravimetric analysis(TV-max??W2+AW3),enthalpy analysis(?H),it can distinguish good quality goods frankincense,falsify frankincense,and incense of the inferior products.Compared with the traditional identification method,identifying frankincense medicinal materials by using TG-DTA thermal analysis method not only can get accurate and reliable results,but also has advantages of using little sample,without pretreatment,no reagents,high sensitivity.3 Qualitative and quantitative research by Infrared spectroscopy of frankincense The experiment apply attenuated total reflection infrared spectroscopy to authenticity identify 41 batch of frankincense samples.Result showed that IR spectra of two batches of frankincense in 41 batches of frankincense have no carbonyl characteristic peak in 1715.75 cm-1,which showed that the two batches of samples are falsify.In addition,our experiment apply near infrared diffuse reflectance infrared spectroscopy and fourier transform attenuated quantitative calibration model for quantitative analysis of content of 11-carbonyl-beta-acetyl frankincense acid in frankincense.In near infrared quantitative model,Calibrating standard deviation(RMSEC)is 0.432,calibrating the correlation coefficient is 0.8443,prediction set standard deviation(RMSEP)was 0.520,prediction set correlation coefficient is 0.9766,11-carbonyl acid-beta,acetyl frankincense error in the range of 0.43?1.07%,the average error of 0.03%.In infrared quantitative model,the calibration set standard deviation(RMSEC)is 0.507,calibrating the correlation coefficient is 0.7773,prediction set standard deviation(RMSEP)for 0.538,correlation coefficient of prediction set to 0.9362,11-carbonyl acid-beta-acetyl frankincense error in the range of 0.73?0.40,the average error of 0.40%.Predict the calibrating the correlation and coefficient set correlation coefficient of each component in quantitative modeltend to 1,the average error is less than 3%,which show that the model accuracy is good.Whereas,near infrared quantitative calibration model compare with the infrared quantitative standard deviation correction model is closer to zero,the correlation coefficient closer to 1,the correlation is stronger,predicted results better,the model is more robus.Conclusion:In this paper,we use two kinds of new technology to qualitify evaluation of frankincense in view of the problem exist in the traditional identification of frankincense such as the large dosage,not objective,time-consuming,on the basis of traditional identification.The results showed that:1.TG-DTA technology,simple operation,which is a rapid,accurate,simple,frankincense,identify new method and can be used as quality analysis.2.Infrared spectroscopy can be used in the identification and the effective composition content of frankincense authenticity of rapid determination,to evaluate the quality of frankincense.In addition,near infrared quantitative calibration model compared to infrared quantitative calibration model,the predicted results of which are more accurate,the model of which is more robust.This topic established the identification method,which is rapid,accurate,simple,and have great significance to quality evaluation of frankincense. |
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