超高效液相色谱-四极杆/线性离子阱质谱法同时测定不同产地何首乌中10种核苷类成分  

Simultaneous Determination of Nucleosides and Nucleobases in Polygoni Multiflori Radix from Different Origins by UPLC-QTRAP-MS/MS

作　　者：罗益远 刘娟秀[1] 刘训红[1] 兰才武 侯娅[1] 马阳[1] 徐力 

机构地区：[1]南京中医药大学药学院,江苏南京210023 [2]贵州昌昊中药发展有限公司研发部,贵州凯里556000 [3]扬州市药品检验所化学室,江苏扬州225000

出　　处：《分析测试学报》2015年第5期519-524,共6页Journal of Instrumental Analysis

基　　金：国家科技支撑计划项目(2011BAI13B04);江苏高校优势学科建设工程资助项目(ysxk-2014)

摘　　要：建立了何首乌药材中10种核苷类成分（尿嘧啶、胞苷、鸟嘌呤、尿苷、腺嘌呤、肌苷、鸟苷、胸苷、腺苷、2＇-脱氧胞苷）的超高效液相色谱-串联四极杆/线性离子阱质谱（UPLC-QTRAP-MS/MS）同时测定的分析方法。不同产地何首乌样品用超纯水在室温下超声提取,提取液经高速离心处理,取上清液,经Waters Atlantis T3色谱柱（2.1 mm×150 mm,3μm）,以甲醇-5 mmol/L醋酸铵（含0.1%冰醋酸）为流动相,0.4 m L/min梯度洗脱,采用正离子多反应监测（MRM）模式测定。10种核苷在一定浓度范围内具有良好的线性关系,相关系数均大于0.99,检出限为1.05~9.68 ng/m L;平均加标回收率为97.8%~104.8%,相对标准偏差（RSD）在1.8%~5.0%之间。该方法简便、灵敏、准确,为何首乌药材内在质量的评价和控制提供了可靠的检测方法。A comprehensive analytical method based on ultra performance liquid chromatography-quadrupole linear ion trap mass spectrometry（ UPLC-QTRAP-MS / MS） was developed for the simultaneous determination of 10 nucleosides and nucleobases（ uracil,cytidine,guanine,uridine,adenine,inosine,guanosine,thymidine,adenosine,2＇-deoxycytidine） in Polygoni Multiflori Radix.The sample was extracted with ultrapure water by ultrasonic machine at room temperature and centrifuged. Under the optimized conditions,good separations for 10 target compounds were obtained on a Waters Atlantis T3column（ 2. 1 mm × 150 mm,3 μm） with a mobile phase of methanol-5 mmol / L ammonium acetate（ 0. 1% acetic acid） at a flow rate of 0. 4 m L / min. The target compounds were analyzed in the positive ion multiple reaction monitoring（ MRM） mode. As a result,10 nucleosides and nucleobases obtained good linearities in the certain concentration ranges with correlation coefficients more than 0. 99,and the limits of detection were in the range of 1. 05-9. 68 ng / m L. Average recoveries of 10 compounds were between 97. 8% and 104. 8%,and the relative standard deviations were between 1. 8% and 5. 0%. The method was simple,sensitive and accurate,and could provide a reliable and effective technique for the quality control of Polygoni Multiflori Radix.

关 键 词：何首乌 超高效液相色谱-串联四极杆/线性离子阱质谱 产地 核苷 碱基 同时测定 

分 类 号：O657.6[理学—分析化学] R282.5[理学—化学]