| Objective:Cataplasm is a commonly used formulation of traditional Chinese medicine preparations.It is widely used modern Chinese medicine preparations especially in TCM Pediatrics and other clinical advantages of disease.However,the TCM cataplasms are usually used sensory and empirical evaluation,which is lack of objective and quantitative evaluation system.In this paper,we applied near-infrared technology,near infrared imaging technology and rheology technology to identify the key quality attributes in the preparation process,analysis the effects of the traditional Chinese medicine system on the cataplasms and determined the key process parameters in the preparation process.Methods:1.Investigation on the quality of commercially available cataplasms(1)We collected 6 kinds of commercial cataplasms with different quality grades as the object of study,using adhesion index to realize the evaluation of commercially available cataplasms.(2)The surface uniformity of the commercially available cataplasms was evaluated by near infrared imaging(NIR-CI)technique.The surface of the commercially available cataplasms was analyzed by the basic correlation analysis method(BACRA).The surface uniformity evaluation of commercially available cataplasms was achieved by statistical calculation results of autocorrelation near infrared imaging spectral correlation.2.The effect of the addition of Chinese herbal extract on the shaping and performance of TCM cataplasms was studied by using near infrared imaging and polymer rheology technology.(1)We concentrated the Chinese herbal extract into the relative density of 1.0 to 1.4 and then cataplasms with Chinese herbal extract of different relative density were prepared.Their adhesion and sensory index were evaluated.(2)The linear viscoelastic region(LVR),complex modulus G*,elastic modulus G ’,viscous modulus G" and so on were determined by rheological technology to study the internal properties of the cataplasms made by adding different Chinese herbal extracts.(3)Near-infrared spectroscopy was performed on the surface of the cataplasms with different relative density of Chinese herbal extract by near-infrared imaging.The near-infrared imaging and the surface spectra data analysis of the cataplasms were used to investigate the surface uniformity of cataplasms.3.Several critical quality attributes in the preparation of TCM cataplasms monitored by near infrared technology(1)The near-infrared imaging(NIR-CI)technology was used to determine the uniformity of the material mixing at different time points.The optimum mixing time during cataplasm preparation was determined.(2)The near infrared spectroscopy(NIR)was used to monitor the cross-linking reaction of the cataplasm matrix in real time.The deviation of the near infrared spectra at different time points was calculated by the standard deviation method(MBSD).The rapid cross-linking reaction time of different prescriptions was determined.The feasibility of determining the end point of crosslinking reaction of cataplasm by near infrared spectroscopy was confirmed by measuring the change rate of gel strength every 24 hours.(3)The degree of cross-linking of the cataplasm was determined by in vitro release study,and the reliability of the cross-linking reaction endpoint was judged by near-infrared spectroscopy,which validated the reliability of near infrared spectroscopy to judge the end point of cross-linking reaction.Results:1.Investigation on the quality of commercially available cataplasms(1)The initial adhesion force and peel strength of kinds of commercial cataplasms were quite different.Research is further derived that the initial adhesion force should stick to the ball(Ruled by Pharmacopoeia)not less than NO.9.Peel strength ranged-0.11N to-0.48 N was qualified,which provided a reference for the quality evaluation of cataplasms made by ourselves.(2)We can see that the visualization of the 6 brands of imaging showed a different degree of uniformity,and the relative standard deviation of the spectral correlation of 6th brand is as high as 23%,indicating whose surface was inhomogeneous.Meanwhile,the relative standard deviation of the 3rd brand was minimum,which was uniform.This method provided technical support for the later use of near infrared imaging technology to judge the surface uniformity of TCM cataplasms.2.The effect of the addition of Chinese herbal extract on the shaping and performance of TCM cataplasms was studied by using near infrared imaging and polymer rheology technology.(1)It was found that the relative density of Chinese medical concrete had a great influence on the cataplasms forming,and the relative density of the Chinese medical concrete could affect the adhesive property and crosslinking strength of the cataplasms.When the relative density of Chinese medical concrete is 1.12,the appearance of the cataplasm is better,no infiltration and the viscosity is better.(2)When the relative density of the extract was 1.12,the complex modulus G*and the linear viscoelastic region(LVR)is large,indicating that the structural strength is large and the structure is stable,showing the "strong gel" characteristics.(3)When the relative density of the Chinese herbal extract was 1.049 and 1.12,the relative standard deviation(RSD)between the surface spectra of the cataplasms was 1%,the surface distribution was more uniform.This method replaced the sensory index observed by the naked eye,resulting in a more standardized and objective evaluation of the traditional Chinese medicine cataplasms.3.Several critical quality attributes in the preparation of TCM cataplasms monitored by near infrared technology(1)When the material was mixed for 20 min,the difference in NIR spectra absorbance between the surface of the cataplasms was the smallest(RSD = 0.01),indicating that the cataplasms had been mixed uniformly.Therefore,it was finally determined that the surface of the cataplasms was more uniform and favorable for coating after the material mixed for 20 min.(2)The near-infrared spectroscopy can monitor about 10%change of the gelatinous intensity.When the change rate of gelatinous intensity was less than 10%within 24h,that was the cataplasm system had entered the slow reaction period,there was no change in the surface spectrum of the cataplasm.By comparing the gelatinous intensity and crosslinking reaction time of cataplasms prepared by different prescriptions,it was found that the effect of each material on the intensity and crosslinking reaction rate of cataplasms.(3)The cumulative release rate of the drugs in 3 prescriptions was the highest at 72h,72h and 120h,respectively.The results showed that the cataplasms of 3 prescriptions were close to the end of the rapid cross-linking reaction.The results of this experiment were consistent with those of the cross-linking reaction endpoints monitored by near-infrared spectroscopy,the near infrared spectroscopy can be used to determine the reliability of the end point of the crosslinking reaction.Conclusion:In this paper,we tried to build a preparation process and finished product quality evaluation method system of TCM cataplasm using a variety of new technologies.We applied near-infrared imaging technique to study the surface uniformity of commercially available and self-made cataplasms,which made the evaluation parameters of cataplasms more accurate and objective.We used rheology technology to study the internal properties of different prescription and found the effect of adding different concentration of Chinese medical concrete on the preparation of cataplasms.The adhesion and viscoelasticity of cataplasms under different prescriptions were compared and the optimal prescription was determined.The key quality parameters in the preparation of cataplasms were monitored by near infrared technique,and the optimal parameter value was obtained.The near-infrared spectroscopy technology was used to monitor the critical quality attributes in the process of cataplasm preparation and the optimal parameter values were found.The methodological system constructed in this paper made the evaluation of TCM cataplasms more accurate and objective,ensuring the quality of cataplasms more uniform,stable and controllable. |
