Quality Analysis And Quality Standard Study Of Pollen Typhae,pollen Typhae With Staminate Flower And Its Decoction Pieces

Objective:Combination quality analysis and the test result on the basis of the legal standard of 134 batches of samples,to control the drug safety and improve the quality standard and unified decoction pieces processing procedures specification as starting points,The exploratory study include illegally dyeing,weight gain,improving decoction pieces quality standards,decoction pieces processing research and heavy metal detection,find out the major problems affecting safety and effectiveness of the variety,and further improve the standardization and effectiveness of the quality standards.Methods:1.According to the legal quality standards?CHP 2015 edition,STMI 2007007and regional standards?,Test Descriptive Information,The micro-identification,Impurity limitation,the water inspection,the total ash inspection of samples,using TLC to identify Typhaneoside and Isorhamnetin-3-O-neohespeidoside,using HPLC to determine total contents of two components.At the same time,TLC,HPLC,HPLC-DAD and HPLC-MS were used to detect the presence of Auramine O in the sample.2.To establish inspection method of Typhae Pollen illegally dyed with Auramine O,tartrazine and metanil yellow.Firstly,TLC was used to preliminary test.Then the results were verified by HPLC-DAD method.Separation was performed on a C18column?150 mm×4.6 mm,5?m?with methyl alcohol as mobile phase A and 0.2mol·L^-1 ammonium acetate as mobile phase B using a gradient elution program?0-10min,10%A,90%B;5-6min,10%A?30%A,70%B?5%B?.The detection wavelengths were 428nm for tartrazine,422nm for metanil yellow and 436nm for Auramine O.HPLC-MS was applied to confirmation with acetonitrile:0.2 mol·L^-1ammonium acetate?35:65?as the mobile phase and positive electrospray ionization as the detection mode.3.Using chemical reaction in the early screening,confirm Ca and Mg by ICP-AES,establish illegal adulterated chemistry examination method of magnesium salt,calcium salt,inspecte illegally adulterated in the sample.4.Through the establishment and determination of the HPLC specific chromatogram of the sample,inspecte the change rule of some chemical substances in the process of pollen typhae and its decoction pieces.5.The methods of TLC,HPLC were used to detecte Typhaneoside and Isorhamnetin-3-O-neohespeidoside of Pollen Typhae with staminate flower in qualitative and quantitative,and verified the methodology.Descriptive Information,The micro-identification,TLC identification,the water inspection,the total ash inspection and HPLC determination of total contents of Typhaneoside and Isorhamnetin-3-O-neohespeidoside in Pollen Typhae with staminate flower were added.At the same time,it also increased the quality control key project Impurity limitation and total ash of three kinds of pollen typhae decoction pieces.6.ICP-MS was used to detect harmful elements in samples include Lead,cadmium,arsenic,mercury and copper.Results:1.134 batches of Pollen Typhae and their decoction pieces were tested according to the current statutory standards and the unqualified rate was 25.4%.The main problems influencing the quality of Pollen Typhae and its decoction pieces included illegal dyeing,illegal weight gain and illegal adulteration.2.10 batches the decoction pieces were stained by auramine O,1 batches was stained by tartrazine,3 batches were stained by tartrazine,tartrazine illegal dyeing was detected for the first time among Pollen Typhae and their decoction pieces,metanil yellow illegal dyeing was first discovered in medicinal materials.In TLC test,three colouring matters could be identified specifically by clear and well separated spots.In HPLC-DAD tes,the retention times and UV spectra of the detected peaks of the test solution corresponded to those of the reference solution.In HPLC-MS test,the molecular ions and fragments of the detected peaks of the test solution corresponded to those of the reference solution.3.The method of illegal weight gain was used to detect,and 4 batches of samples were found to gain weight with magnesium salt and calcium salt.4.These added items of Pollen Typhae with staminate flower and three Typhae Pollen decoction pieces can effectively reflect their quality situation.The sports were fairly clear and visible in TLC of Pollen Typhae with staminate flower,The contents of Typhaneoside and Isorhamnetin-3-O-neohespeidoside showed a good linear relationship in the range of 0.048⁰.951?g?r=0.9999?and 0.046⁰.920?g?r=0.9999?,respectively.The average recoveries were 99.06%with RSD of 1.25%and 98.23%with RSD of 1.40%,respectively.5.In 14 batches samples,lead,cadmium,arsenic,mercury and copper were found to be on the high side,indicating possible safety risks.Conclusion:1.In general,the quality of Pollen Typhae,Pollen Typhae with staminate flower and its decoction pieces was poor.The qualified rate of the approved sample was74.6%,and the qualified rate was 67.2%according to the standard study.The main problems included illegal dyeing,illegal weight gain and illegal adulteration.There was a tendency of using many kinds of dyeing agents for illegal dyeing.2.The determination method of three colouring matter have be approved by China Food and Drug Administration,and used as a formal standard execution?supplement Numbers:BJY201803?on January 15,2018.3.The revised standard is accurate,effective and can be usd to control the quality of Pollen Typhae with staminate flower and Typhae Pollen decoction pieces.4.In A few samples,lead,cadmium,arsenic,mercury and copper were found to be on the high side,indicating that the growth environment of medicinal materials is still possible,but there may be safety risks.