Study On Quality Control And Evaluation System Of Pudilan Xiaoyan Tablets

Objective Pudilan Xiaoyan Tablets have many manufacturers,different production processes,inconsistent quality standards and single test items.In order to construct a complete quality control and evaluation system,and provide reference for perfecting and improving the quality standard of Pudilan Xiaoyan tablets,we conducted an exploratory study on the authenticity,safety and effectiveness of Pudilan Xiaoyan tablets.Methods 1.48 batches of Pudilan Xiaoyan tablets were tested according to the current quality standard.2.The TLC method was used to qualitatively identify the corresponding reference herbs and their main active ingredients.3.The ICP-MS method was used for the simultaneous determination of lead,cadmium,arsenic,mercury and copper,and the safety was evaluated by single pollution index method and Nemerow comprehensive pollution index methods.4.The UPLC method was established to rapidly screen 5 kinds of yellow pigments including tartrazine,sunset yellow,orange Ⅱ,auramine O and acid yellow 36 in Pudilan Xiaoyan tablets.5.The HPLC fingerprints of Pudilan Xiaoyan tablets was established and the similarity was evaluated,and the evaluation model was established combined with chemical pattern recognition.6.The relative correction factors of caftaric acid,cichoric acid,wogonoside,baicalein and wogonin were established using baicalin as the internal reference,and the difference between the Quantitative Analysis of Multi-components by Singlemarker and the external standard method was compared by the relative error method.Results 1.According to the current quality standards,48 batches of Pudilan Xiaoyan tablets were in compliance.2.The TLC method is accurate and reliable,easy to operate,with moderate Rf value and clear TLC spots.3.The linear relationships of 5 kinds of heavy metals and harmful elements were good(r>0.999),and the recoveries were 87.6%-105.7%.Referring to the relevant limit standards of the Green Industry Standard for Import and Export of Medicinal Plants and Preparations,the arsenic content of 7 batches of samples exceeded the limit values.The order of the average single pollution index was As>Cu>Cr>Hg>Pb,the Nemerow comprehensive pollution index was 0.09～0.97,and most samples were at the safety level.4.The separation,specificity and linearity of the five yellow pigments were good(r>0.999),the precision RSD was 0.14%～1.3%,the accuracy test recoveries were 99.9%～103.9%,the limits of detection(LOD)were 0.12～1.2ng,and no positive samples were detected in 48 batches of samples.5.The HPLC fingerprints were established by wavelength switching method,14 common peaks were determined,8 of them were identified,and the peaks were attributed to the herbs.The similarities of the 48 batches of samples were all greater than 0.9,the samples were grouped into 3 categories by cluster analysis,principal component analysis and orthogonal partial least squares-discriminant analysis,and 6 different components were screened out.6.The relative correction factors of caftaric acid,cichoric acid,wogonoside,baicalein and wogonin relative to baicalin were 1.1281,0.9097,0.8982,0.7033 and 0.6101 respectively.The RSD was less than 3%under different chromatographic conditions,and the relative error method was used to compare the QAMS method and ESM method,and the relative error of each component was less than 5%.Conclusion 1.The established ICP-MS method for five heavy metals and harmful elements and UPLC method for five yellow pigments can accurately and efficiently analyze the heavy metal residues and pigment staining in Pudilan Xiaoyan tablets.2.The established HPLC fingerprint method based on chemical identification mode is scientific and reliable,which can provide accurate information for the identification and analysis of the active ingredients in Pudilan Xiaoyan tablets,and provide a basis for the comprehensive evaluation and control of the quality of the relevant preparations.3.The established QAMS method for the determination of the content of multi-indicator components is accurate and reliable,which can effectively solve the problem of high testing cost caused by the difficulty in obtaining the control and the high price.