15:15-15:35 陈长兰-微波法虫草素提取
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微波消解-ICP-MS法测定青海和西藏产区冬虫夏草中的35种元素张敏敏;赵恒强;赵志国;刘伟;刘倩;梁琰;耿岩玲;黄璐琦;王晓【摘要】To determine the contents of 35 elements(including 16 rare earth elements)in 17 batches of Chinese caterpillar fungus from Qinghai and Tibet and make preliminary identification analysis of their habitats,a total of 35 elements in Chinese caterpillar fungus samples were determined by microwave digestion-ICP-MS,including 3 batches from Yushu,4 batches from Naqu and 10 batches from Guoluo.Furthermore,cluster analysis was carried out on the measurement results of 3 producing areas. Results showed that the contents of 35 elements in 17 kinds of Chinese caterpillar fungus samples from different origins have obvious differences. And the limits of the 4 kinds of harmful elements(Cd,Pb,As and Cu) were recommended. The results of cluster analysis showed that the samples from Yushu and Guoluo were close,and the difference was small,while the sample from Naqu was far away,and its relative difference was larger. This method is quick,accurate and feasible,which provides a theoretical basis for quality control and medication guidance of Chinese caterpillar fungus from different habitats.%为了测定青海和西藏产区的17批冬虫夏草中的35种元素(其中16种为稀土元素)的含量,并进行初步产地鉴别分析,运用微波消解-ICP-MS法测定了3批玉树、4批那曲和10批果洛产区的虫草样本,并对3个产区的测定结果进行聚类分析.结果表明,不同产区的虫草药材各种元素含量差别较大,本文对其中4种有害元素Cd,Pb,As,Cu推荐了限量标准;聚类分析结果表明,玉树和果洛产区聚类较近、差异性较小;那曲产区聚类较远,相对差异性较大.该方法快捷、准确、可行性强,为不同产地冬虫夏草药材的质控和用药安全指导提供了理论依据.【期刊名称】《山东科学》【年(卷),期】2017(030)005【总页数】7页(P14-20)【关键词】ICP-MS;冬虫夏草;微量元素;稀土元素【作者】张敏敏;赵恒强;赵志国;刘伟;刘倩;梁琰;耿岩玲;黄璐琦;王晓【作者单位】山东省中药质量控制技术重点实验室,山东省科学院中药过程控制研究中心,山东省分析测试中心,山东济南250014;山东省中药质量控制技术重点实验室,山东省科学院中药过程控制研究中心,山东省分析测试中心,山东济南250014;山东省中药质量控制技术重点实验室,山东省科学院中药过程控制研究中心,山东省分析测试中心,山东济南250014;山东省中药质量控制技术重点实验室,山东省科学院中药过程控制研究中心,山东省分析测试中心,山东济南250014;山东省中药质量控制技术重点实验室,山东省科学院中药过程控制研究中心,山东省分析测试中心,山东济南250014;山东省中药质量控制技术重点实验室,山东省科学院中药过程控制研究中心,山东省分析测试中心,山东济南250014;山东省中药质量控制技术重点实验室,山东省科学院中药过程控制研究中心,山东省分析测试中心,山东济南250014;中国中医科学院中药资源中心,道地药材国家重点实验室培育基地,中国中医科学院,北京100700;山东省中药质量控制技术重点实验室,山东省科学院中药过程控制研究中心,山东省分析测试中心,山东济南250014【正文语种】中文【中图分类】R284.1Ab stract∶To determine the contents of 35 elements (including 16 rare earth elements) in 17 batches of Chinese caterpillar fungus from Qinghai and Tibet and make preliminary identification analysis of their habitats, a total of 35 elements in Chinese caterpillar fungus samples were determined by microwave digestion-ICP-MS, including 3 batches from Yushu, 4 batches from Naqu and 10 batches from Guoluo. Furthermore, cluster analysis was carried out on the measurement results of 3 producing areas. Results showed that the contents of 35 elements in 17 kinds of Chinese caterpillar fungus samples from different origins have obvious differences. And the limits of the 4 kinds of harmful elements (Cd, Pb, As and Cu) were recommended. The results of cluster analysis showed that the samples from Yushu and Guoluo were close, and the difference was small, while the sample from Naqu was far away, and its relative difference was larger. This method is quick, accurate and feasible, which provides a theoretical basis for quality control and medication guidance of Chinese caterpillar fungus from different habitats.Key words∶ICP-MS;Chinese caterpillar fungus; trace elements; rare earth elements冬虫夏草又称虫草,为麦角菌科真菌冬虫夏草菌Cordyceps sinensis (Berk. ) Sacc. 寄生在蝙蝠蛾科昆虫幼虫上的子座和幼虫尸体的干燥复合体[1]。
HPLC测定祁连产冬虫夏草中虫草素和虫草酸的含量汪陈才(2008 B,青海师范大学,化学系)摘要为建立一种有效的利用高效液相色谱法(HPLC)测定冬虫夏草中虫草素和虫草酸含量的方法,用甲醇超声提取虫草素、水超声提取虫草酸,再利用高效液相色谱、示差折光检测器和紫外检测器分别测定冬虫夏草中虫草素和虫草酸含量。
通过对样品进行预处理,色谱条件和方法指标的验证,建立了定量检测虫草中虫草素和虫草酸的一种有效方法,二者精密度( RSD) ≤1.77% 。
虫草素、虫草酸检出限为50 ng/mL 和1.5 μg/mL。
测得样品中虫草素和虫草酸的平均组分含量为0.258mg·g-1和79.7mg·g-1二者回收率在93.7%~98.4%之间。
该方法具有快速、准确、简便的特点。
关键字: 高效液相色谱虫草虫草素虫草酸Abstract:A high performance liquid chromatographic (HPLC) with diode- array detector (DAD) and refractive index detector ( RID) method for the determination of cordycepin and cordycep acid in cordyceps sinensis was studied. Both of it were extracted by Methanol and water with Ultrasonic wave. Then by using high performance liquid chromatography, refractive index detector and a UV detector were measured in Cordyceps and cordycepic acid content. Based on the sample pretreatment, chromatographic conditions and method validation, establishes the quantitative detection of cordycepin and cordycepic acid is an effective method. Their precision (RSD) were lower than 1.77%. The samples of cordycepin and cordycep acid content averages are 0.258 mg•g1and 79.7mg•g-1. Their recovery were between 91.9% and 93.7%. The method is rapid, accurate and simple features.Key words HPLC; Cordyceps sinensis; Cordycepin; Cordycep acid冬虫夏草(Cordyceps Sinensis)与人参、鹿茸齐名,为中国三宝之一。