The Research On Quality Standards Of Mylabris Herbs And Pieces

Objective : This program is studying on the processing technology of Mylabris stir-frying with rice and the quality standards of Mylabris,unprocessed Mylabris,Mylabris (stir-frying with rice).We established the determination method of cantharidin and total cantharidin, and compare the changes of content about cantharidin and total cantharidin in the different processed samples , which select the best processing conditions of Mylabris(stir-frying with rice).Determinated the content of trace elements in Mylabris herbs and pieces, and deduced the presence forms of bound cantharidin.We make the quality standards of Mylabris,unprocessed Mylabris,Mylabris (stir-frying with rice),in order to control the quality of Mylabris herbs and pieces.Methods:On the foundation of looking up ancient and modern document,we wrote summaries; Through compared the changes of rice colour and tempature, using infrared thermometer, when Mylabris processed with hand-frying and electric frying,we determined the processing conditions of Mylabris frying with rice; We established the cantharidin HPLC determination method and took the methodological study;Using HPLC method to replace the GC method ,we determined the cantharidin content to optimize the extraction process of it;Compared the changes of the cantharidin content in Mylabris,unprocessed Mylabris,Mylabris (stir-frying with rice) , Mylabris processed by sodium hydroxide and head, legs, inside and outside wings of Mylabris;The total cantharidin content as the index, using orthogonal, we optimized the extraction process of total cantharidin, and established the total cantharidin HPLC determination method; Compared the changes of the total cantharidin content in Mylabris,unprocessed Mylabris,Mylabris (stir-frying with rice) and head, legs, inside and outside wings of Mylabris;We collected Mylabris,unprocessed Mylabris,Mylabris (stir-frying with rice) samples of 10 batches of above;In accordance with the "traditional Chinese medicine quality standards guiding principles",we respectively studied Mylabris pieces name, processing methods, properties, identification, examination and determination, dosage other items, to establish the quality standards of Mylabris,unprocessed Mylabris,Mylabris (stir-frying with rice), and provide drafting instructions;Used graphite furnace, flame, hydride generation atomic absorption spectrometry to determine the content of copper (Cu), manganese (Mn), zinc (Zn), iron (Fe), magnesium ( Mg), calcium (Ca), potassium (K), lead (Pb), cadmium (Cd), arsenic (As), mercury (Hg) and other trace elements in Mylabris herbs and pieces.Results: We wrote two summaries:"The research on Chinese medicine processing by rice in history ";"The research progress of Mylabris processing technology and pharmacological ".We determined the processing conditions of Mylabris frying with rice,wrote standard operating procedures of Mylabris (stir-frying with rice), by the Zhejiang University of Chinese Medicine Chinese Herbal Medicine Factory to produce 9 batches of samples; We choose the chromatographic conditions of cantharidin HPLC determination method:the mobile phase was methanol-water (23:77),the column temperature was 35℃;the flow rate was 1.0 ml?min-1;the detection wavelength was 230 nm;We determined the extraction process of cantharidin as: use chloroform as disslovent, ultrasonicate ( power, not less than 400w; frequence, not less than 40kHZ) 2 times (30 ml, 30 ml), 15 minutes per time, the extraction process of total cantharidin as: A1B2C2D1, take 10 ml of each of chloroform and hydrochloric acid solution(PH=1), ultrasonicate ( power, not less than 400w; frequence, not less than 40kHZ) for 15 minutes; Mylabris containing cantharidin 0.68% (large Mylabris), 0.72% (small Mylabris), with the total cantharidin 1.98% (large Mylabris), 2.34% (small Mylabris); unprocessed Mylabris containing cantharidin 0.79% (large Mylabris) , 0.74% (small Mylabris), with the total cantharidin 2.86% (large Mylabris), 3.55% (small Mylabris); Mylabris (stir-frying with rice) containing cantharidin 0.46% (large Mylabris), 0.32% (small Mylabris), with the total cantharidin 1.30% (large Mylabris), 1.45% (small Mylabris); Mylabris processed by sodium hydroxide containing cantharidin 1.98%; The head, legs, inside and outside wings of Mylabris containing cantharidin 0.16%,with the total cantharidin 0.61% , howerver,the weight of theirs were 28.2%,leading to the contents in Mylabris were lower than unprocessed Mylabris in the same weight.We identified the collected 10 batches of samples on the physical and chemical , microscopic and TLC, detemined moisture content, ash content, insoluble ash content in acid, extract content; HPLC for the determination of cantharidin, Mylabris contains not less than 0.50% of cantharidin (C10H12O4); Unprocessed Mylabri contains not less than 0.65% of cantharidin (C10H12O4);Mylabris (stir-frying with rice) contains not more than 0.65% of cantharidin (C10H12O4), and not less than 1.0% of total cantharidin, calculated as cantharidin (C10H12O4); We determinated 11 trace elements content in the Mylabris samples from high to low were: K> Mg> Fe> Ca> Zn> Mn> Cu> Pb> As> Hg> Cd,but As, Hg, Pb content in Mylabris were highest, Mylabris (stir-frying with rice) minimum;Cd, K, Zn content in unprocessed Mylabris highest, the head, legs, inside and outside wings minimum; Cu, Mg content in Mylabris (stir-frying with rice) highest, the head, legs, inside and outside wings minimum; Mn content in Mylabris highest, Mylabris (stir-frying with rice) and the head, legs, inside and outside wings ,were around, minimum; Fe content in Mylabris highest ,Mylabris (stir-frying with rice) minimum; Ca content in the head, legs, inside and outside wings highest ,unprocessed Mylabris minimum.Conclusion: Standard operating procedures of Mylabris (stir-frying with rice) in this study, from Zhejiang University of Chinese Medicine Chinese Herbal Medicine pilot plant production,was proved feasible strong;Established cantharidin HPLC determination method, better than the 2005 edition Pharmacopoeia GC method ,was highly accurate and reproducible; The cantharidin content of Mylabris after be processed decreased, to provide experimental basis for processing reducing toxicity; The cantharidin content of the head, legs, inside and outside wings were low,so they cannot be used as medicine; Established the quality standards of Mylabris,unprocessed Mylabris,Mylabris (stir-frying with rice)and the drafting instructions,through the Henan Institute for Drug Control review, were collected by "Chinese Pharmacopoeia" 2010 version, to provide a scientific basis for ensure that Chinese medicine clinical drug safe and effective, but also provide a pieces quality standard to company.In Mylabris after be processed, the content of Pb, As, Hg, Cd, Fe elements decrease, Cu, Mg, Ca increased; In the head, legs, inside and outside wings of Mylabris, the content of As, Hg, Pb, Fe elements higher than the other positions, while Cu, Mg, Mn, Zn, K elements was lower, indicating the traditional processing methods, stir-frying with rice and removing head, legs and wings, were scientific.This study proved that Mylabris not only contain free cantharidin more than 0.35% which extracted by chloroform, but also contains bound cantharidin;This is the first to establish the total cantharidin determination method can be used to determine and control the total cantharidin content; Comparee the content of total cantharidin with trace elements, prompting the forms of bound cantharidin likely be cantharidin magnesium, potassium and a small amount of cantharidin zinc exists, for further development provide an experimental basis.