OBJECTIVETo establish the HPLC chromatographic fingerprint of Kumu injection and to simultaneously determine the contents of three beta-carboline alkaloids, comprehensively evaluating the immanent quality of Kumu injection.

METHODThe chromatographic analysis was performed on a Phenomenex Gemini C18 ( 4.6 mm x 250 mm, 5 microm) column with the gradient elution solvent system composed of methanol and 30 mmol x L(-1) aqueous ammonium acetate (adjusted with glacial acetic acid to pH 4.5). Similarity evaluation system for chromatographic fingerprint of traditional Chinese medicine (2004 A) was used in data analysis.

RESULTSixteen co-possessing peaks were selected as the fingerprints of Kumu injection, and 7 peaks were identified by chemical reference substances. There were good similarities between the standard fingerprint chromatogram and each fingerprint chromatogram from the eleven samples for their similarity coefficients were not less than 0.9. Three kinds of beta-carboline alkaloids were separated well. The correlation coefficients were 0.999 9. The linear ranges of three components were 0.020 0-0.300 0, 0.102 0-1.530 0, 0.015 2-0. 228 0 microg, respectively, and the average recoveries ranged were from 99.5% to 102%.

CONCLUSIONThe method of fingerprint combined with quantitative analysis is sensitive, selective, and provide scientific basis for quality control of Kumu Injection.

Alkaloids ; analysis ; Carbolines ; analysis ; Chromatography, High Pressure Liquid ; methods ; Drug Stability ; Drugs, Chinese Herbal ; chemistry ; Injections ; Pharmaceutical Solutions ; Picrasma ; chemistry ; Plants, Medicinal ; chemistry ; Quality Control ; Reproducibility of Results ; Sensitivity and Specificity

OBJECTIVE：To provide reference for improving the quality sta ndard of Equisetum hyemale . METHODS ：Totally 10 batches of E. hyemale from different sites were collected as samples. TLC method was used to qualitatively identify kaempferol- 3-O-β-sophoroside. The contents of heavy metal ，aflatoxin，impurity，moisture，total ash ，acid-insoluble ash ，water-soluble extract and ethanol-soluble extract were determined according to supplementary provisions of Chinese Pharmacopoeia （2015 edition）. HPLC method was used to determine the content of kaempferol- 3-O-β-sophoroside in sample. HPLC fingerprint of water-soluble extract from E. hyemale was also established. RESULTS ：TLC identification showed that in the chromatogram of the test sample ， fluorescent spots with the same color were displayed on the corresponding positions of the chromatogram of substance control of kaempferol-3-O-β-sophoroside，and without interference from blank control. Among 10 batches of samples ，the contents of impurities were 0.19％-2.32％；the water contents were 10.12％-11.87％；the total ash contents were 6.67％-10.11％；the acid-insoluble ash contents were 1.34％-2.12％；the water-soluble extract contents were 9.17％-13.99％；the ethanol-soluble extract contents were 7.49％-13.68％，respectively. It is preliminarily proposed that the impurity content shall not exceed 3.00％；the total ash content shall not exceed 10.00％；the acid-insoluble ash content shall not exceed 2.50％；the water-soluble extract content shall not be less than 9.00％ ；the ethanol-soluble extract content shall not be less than 5.00％. Arsenic（0.064-0.225 mg/kg） 010815） was detected in 9 batches of samples ；cadmium（0.106-0.132 E-mail：cruise0303@163.com mg/kg）was detected in 6 batches of samples ；lead（0.221- 1.896 mg/kg）was detected in all samples ，but no mercury or rebecca aflatoxin was detected. The results of HPLC method met the relevant requirements of Chinese Pharmacopoeia . The content of kaempferol- 3-O-β-D-sophoroside in 10 batches of samples was 627.12-5 384.53 mg/kg，and the similarity of HPLC fingerprints of 10 batches of samples was more than 0.900. CONCLUSIONS ： A new qualitative and quantitative analysis method for kaempferol- 3-O-β-D-sophoroside was established ；the heavy metals ， aflatoxins，impurities and other items in E. hyemale were detected ；the limits of impurity ，ash and extract were determined. The established method is simple ，accurate and reproducible ，and can be used for quality control of E. hyemale .