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作 者:邓双炳 徐滢 黄冰峰 刘明颖 李瑶芳 廖小菁 方礼 刘地发 DENG Shuangbing;XU Ying;HUANG Bingfeng;LIU Mingying;LI Yaofang;LIAO Xiaojing;FANG Li;LIU Difa(State Key Laboratory of Innovative Natural Medicine and TCM Injections,Ganzhou,Jiangxi 341000,China;Jiangxi Qingfeng Pharmaceutical Co.Ltd.,Ganzhou,Jiangxi 341000,China)
机构地区:[1]创新天然药物与中药注射剂国家重点实验室,江西赣州341000 [2]江西青峰药业有限公司,江西赣州341000
出 处:《今日药学》2021年第5期357-360,365,共5页Pharmacy Today
基 金:江西省科技计划项目(JXKJ-CXPT-2016005)。
摘 要:目的基于苦木生物碱类化合物结构特征,建立凯氏定氮法测定总生物碱含量。方法用80%乙醇提取,浓缩干燥后用2%盐酸富集;消解后用凯氏定氮法测定氮原子含量,再换算成以苦木酮计的总生物碱含量。结果苦木提取液中采用鉴别法未检出氨基酸、蛋白质。重复性试验平均含量为1.17%,RSD为2.2%(n=6),中间精密度平均含量为1.19%,RSD为2.6%(n=12)。回收率试验结果在99.5%~105.8%,RSD为1.7%~2.1%。结论该方法的专属性、精密度、准确度、耐用性良好,可用于测定苦木总生物碱的含量。OBJECTIVE To establish a more scientific and accurate Kjeldahl method for the determination of total alkaloids from Picrasma quassioides(PQ),based on the structural characteristics of alkaloids. METHODS The sample of PQ was extracted with 80% ethanol, concentrated and dried, and then 2% hydrochloric acid was used to enrich alkaloid components.After digestion, the nitrogen atoms were determined by Kjeldahl method.According to the amount of sulfuric acid titrant consumed, the amount of nitrogen atoms were calculated, and then converted into the total alkaloid content calculated by the nigakinone. RESULTS The results showed that no amino acid and protein were detected in the sample solution extracted.The average content of repeatability test was 1.17%,RSD was 2.2%(n=6).And the average content of intermediate precision was 1.19 %,RSD was 2.6%(n=12).The recovery ranged from 99.5% to 105.8%,and the RSD was 1.7% to 2.1%. CONCLUSION The method are good specificity, precision, accuracy and durability.It can be used to determine the content of total alkaloids in PQ.
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