1.Study on Improvement of Quality Standard of Equisetum hyemale
Zhengquan LAI ; Weipeng AI ; Zhen HU ; Yaoxing DOU ; Yufeng CAI ; Wei LIU ; Ying WU ; Citing ZHANG ; Xiaolin XIE ; Huijun LIAO
China Pharmacy 2020;31(9):1080-1085
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 .