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采用基质固相分散萃取和高效液相色谱法同时测定冬虫夏草及其替代品中的核苷及其碱基。

Simultaneous determination of nucleosides and their bases in Cordyceps sinensis and its substitutes by matrix solid-phase dispersion extraction and HPLC.

机构信息

College of Chemistry, Jilin University, Changchun, PR China.

出版信息

J Sep Sci. 2013 Jul;36(14):2348-57. doi: 10.1002/jssc.201300204. Epub 2013 Jun 21.

Abstract

Nine nucleosides and nucleobases, including uracil, adenine, thymine, uridine, adenosine, thymidine, cytidine, guanosine, and cordycepin in natural Cordyceps sinensis, cultured Cordyceps mycelia, and Cordyceps fruiting bodies were extracted by matrix solid-phase dispersion (MSPD) and determined by HPLC. The experimental conditions for the MSPD extraction were optimized. Florisil was used as dispersant, petroleum ether as washing solvent, and methanol as elution solvent. The Florisil-to-sample ratio was selected to be 4:1 and no additional clean-up sorbent was needed. The calibration curves had good linear relationships (r > 0.9997). The LOD and LOQ were in the range of 12~79 and 41~265 ng/mL, respectively. The intra- and interday precision were lower than 8.3%. The recoveries were between 61.5 and 93.2%. The present method consumed less sample compared with ultrasonic extraction and heating reflux extraction (HRE). The extraction yields obtained by using the present method are much higher than those obtained by UE and comparable to those obtained by HRE.

摘要

从天然冬虫夏草、冬虫夏草菌丝体和冬虫夏草子实体中提取了 9 种核苷和碱基,包括尿嘧啶、腺嘌呤、胸腺嘧啶、尿苷、腺苷、胸苷、胞苷、鸟苷和蛹虫草素,并用高效液相色谱法进行了测定。通过基质固相分散(MSPD)提取的实验条件进行了优化。弗罗里硅土被用作分散剂,石油醚作为洗涤溶剂,甲醇作为洗脱溶剂。弗罗里硅土与样品的比例选择为 4:1,无需额外的净化吸附剂。校准曲线具有良好的线性关系(r>0.9997)。LOD 和 LOQ 分别在 12~79 和 41~265ng/mL 范围内。日内和日间精密度均低于 8.3%。回收率在 61.5%至 93.2%之间。与超声提取和加热回流提取(HRE)相比,本方法消耗的样品更少。与 UE 和 HRE 相比,本方法的提取收率要高得多。

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