| Cinnamomi Cortex is the dried bark of Cinnamomum cassia Presl.Cinnamomi Cortex contains volatile oil,polyphenols,flavanols and terpenes and other chemical components,with anti-inflammatory,anti-pathogenic microorganisms,improve glucose and lipid metabolism,immune regulation and anti-tumor pharmacological effects.China is mainly produced in Guangdong,Guangxi and other provinces,the Chinese medicine is also one of the important spices and medicinal materials in the world.Objective:Under the guidance of traditional Chinese medicine theory and modern analytical methods,study on Cinnamomi Cortex medicinal materials,starting from two aspects of chemical analysis and pharmacodynamic activity research,throw the high performance liquid chromatography and near infrared spectrophotometry,combined with chemometrics methods to clarify the pharmacodynamic material basis of Cinnamomi Cortex,establishment of comprehensive overall quality evaluation system,systematic evaluation of the quality of Cinnamomi Cortex,provide the new ideas and methods for quality control of Cinnamomi Cortex.Methods:(1)Study on fingerprint of Cinnamomum cassia based on chemometrics method: HPLC method was used,the chromatographic column was Waters XBridge C18(250 mm×4.6 mm,5 μm);mobile phase: acetonitrile-0.1 %phosphoric acid aqueous solution(gradient elution: 0-20 min 24 % A,20-21 min 24 %-27 % A,21-35 min 27 %-35 % A);flow rate is 1.0 m L/min,detection wavelength was 250 nm,column temperature was 25 ℃.After the fingerprints of Cinnamomum cassia from different areas were established,three chemometric methods including principal component analysis,cluster analysis and orthogonal partial least squares analysis were used for statistical analysis.(2)Study on spectrum-effect relationship of Cinnamomum cassia:establishment of mouse model of kidney-yang deficiency by intragastric administration of hydrocortisone,preliminary study on the effect and mechanism of Cinnamomi Cortex on kidney-yang deficiency by hypothalamus-pituitary-thyroid(HPT)axis function and hypothalamus-pituitary-adrenal-thymus(HPAT)axis function,analysis of chemical constituents and pharmacodynamic indexes represented by common peaks in fingerprint by grey correlation degree method,study on pharmacodynamic material basis of Cinnamomi Cortex in improving kidney-yang deficiency.(3)Study on quality control of Cinnamomum cassia based on one measurement and multiple evaluation: relative correction factors(f)of coumarin,cinnamic alcohol,cinnamic acid and O-methoxy cinnamaldehyde were determined with cinnamic aldehyde as internal reference,calculation of its content by f,and the measured values were compared with the measured results by external standard method.(4)Rapid quantitative analysis of volatile oil in Cinnamomum cassia based on near infrared spectroscopy: GC-MS method was used,the chromatographic column was HP-5MS(30 m × 0.25 mm × 0.25 μm),the temperature programming was performed,the injection volume was 1 μL,the split ratio was 30: 1,the carrier gas was high purity He,the carrier gas flow rate was 1.0 m L/min,the EI source temperature was 230 ℃,the interface temperature was 280 ℃,and the scanning mass range was 35-550 aum,content determination method using internal standard method,methyl salicylate as internal standard.Combined with the determination results of Cinnamomi Cortex volatile oil content,a rapid quantitative analysis method of Cinnamomi Cortex volatile oil was established by near infrared spectroscopy.Results:(1)Study on fingerprint of Cinnamomum cassia based on chemometrics method: the fingerprints of 27 batches of Cinnamomi Cortex from different habitats were established,and six common peaks were calibrated.Under the common mode,five peaks of coumarin,cinnamic alcohol,cinnamic acid,cinnamic aldehyde and O-methoxy cinnamaldehyde were identified by reference substance comparison method.No.1、2、3、5、6、7 were selected as the index components for cluster analysis,principal component analysis and orthogonal partial least squares analysis.The results showed that Guangxi and Guangdong were significantly different from the medicinal materials of Cinnamomi Cortex from Vietnam.It is suggested that coumarin,cinnamic alcohol,cinnamic acid,cinnamaldehyde and O-methoxy cinnamaldehyde may be the quality markers of Cinnamomi Cortex in three regions(2)Study on spectrum-effect relationship of Cinnamomum cassia:correlation between HPLC fingerprint and improvement of kidney yang deficiency by grey correlation analysis.The results showed that cinnamic acid in Cinnamomi Cortex water decoction was a component with high correlation(r > 0.74).The correlation between cinnamic aldehyde and cinnamic acid was the highest in the methanol extract of Cinnamomi Cortex(r > 0.80),and the correlation between O-methoxy cinnamaldehyde was the highest(r > 0.72).In this study,according to the correlation degree,the contribution degree of each component in Cinnamomi Cortex extract to the improvement of kidney yang deficiency was determined.Cinnamic aldehyde,cinnamic acid and O-methoxy cinnamaldehyde were preliminarily confirmed as the pharmacodynamic material basis of Cinnamomi Cortex.(3)Study on quality control of Cinnamomum cassia based on one measurement and multiple evaluation: simultaneous determination of five components in 70 batches of Cinnamomi Cortex from different habitats by high performance liquid chromatography combined with one-time quantitative analysis.Among them,there was no significant difference in the content determination results of cinnamic alcohol,cinnamic acid,cinnamic aldehyde and O-methoxy cinnamaldehyde by one-time multi-assessment method compared with those by external standard method.(4)Rapid quantitative analysis of volatile oil in Cinnamomum cassia based on near infrared spectroscopy: near-infrared spectroscopy combined with chemometrics was used to determine and analyze the volatile oils from multiple batches of Cinnamomi Cortex from different habitats,and a relatively reliable and adaptable model for quantitative analysis of five index components was established,average relative deviations of prediction values of borneol,cinnamic aldehyde,cinnamic alcohol,cinnamic acid and O-methoxy cinnamaldehyde were less than 5 %,average relative deviation of prediction value of coumarin is greater than 5 %,it suggested that the prediction results of borneol,cinnamic aldehyde,cinnamic alcohol,cinnamic acid and O-methoxy cinnamaldehyde were accurate and the modeling was successful;the prediction results of coumarin have large deviation and fail to establish an accurate model.Conclusion : The present study set up high performance liquid chromatography fingerprint of Cinnamomi Cortex in different areas,quality control of Cinnamomi Cortex from different sources in the market based on the integrity and fuzziness of fingerprint;analysis of spectral effect correlation between fingerprint and improvement of kidney-yang deficiency symptoms by grey correlation degree method,the experimental design of material basis for studying the effect of Cinnamomi Cortex on improving kidney-yang deficiency is reasonable and the results are reliable;a HPLC method for the determination of cinnamic alcohol,cinnamic acid,cinnamic aldehyde and O-methoxy cinnamaldehyde in 70 batches of Cinnamomi Cortex from different habitats was established,the method is rapid,simple and accurate.In this study,near infrared spectroscopy combined with chemometric methods were used to determine and analyze the volatile oil of Cinnamomi Cortex from different origins,a relatively reliable and adaptable quantitative model for 4 index components was also established.In conclusion,this study preliminarily clarified the pharmacodynamic material basis of Cinnamomi Cortex,established the quality evaluation system of Cinnamomi Cortex,and provided ideas and methods for the quality evaluation and control of Cinnamomi Cortex. |
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