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Fast Simultaneous Determination of 13 Nucleosides and Nucleobases in Cordyceps sinensis by UHPLC-ESI-MS/MS

机译:用UHPLC-ESI-MS / MS快速同时测定冬虫夏草中13种核苷和核糖核酸酶

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摘要

A reliable ultra-high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UHPLC-ESI-MS/MS) method for the fast simultaneous determination of 13 nucleosides and nucleobases in Cordyceps sinensis (C. sinensis) with 2-chloroadenosine as internal standard was developed and validated. Samples were ultrasonically extracted in an ice bath thrice, and the optimum analyte separation was performed on an ACQUITY UPLCTM HSS C18 column (100 mm x 2.1 mm, 1.8 m) with gradient elution. All targeted analytes were separated in 5.5 min. Furthermore, all calibration curves showed good linear regression (r > 0.9970) within the test ranges, and the limits of quantitation and detection of the 13 analytes were less than 150 and 75 ng/mL, respectively. The relative standard deviations (RSDs) of intra- and inter-day precisions were <6.23%. Recoveries of the quantified analytes ranged within 85.3%-117.3%, with RSD < 6.18%. The developed UHPLC-ESI-MS/MS method was successfully applied to determine nucleosides and nucleobases in 11 batches of C. sinensis samples from different regions in China. The range for the total content in the analyzed samples was 1329-2057 mu g/g.
机译:一种可靠的超高效液相色谱-电喷雾电离串联质谱(UHPLC-ESI-MS / MS)方法,以2-氯腺苷为内部成分,可快速同时测定冬虫夏草(C. sinensis)中13种核苷和核苷碱基标准已开发并验证。将样品在冰浴中超声提取三次,然后在ACQUITY UPLCTM HSS C18色谱柱(100 mm x 2.1 mm,1.8 m)上以梯度洗脱进行最佳分析物分离。 5.5分钟内分离所有目标分析物。此外,所有校准曲线在测试范围内均表现出良好的线性回归(r> 0.9970),对13种分析物的定量和检测极限分别小于150 ng / mL和75 ng / mL。日内和日间精度的相对标准偏差(RSD)<6.23%。定量分析物的回收率在85.3%-117.3%之间,RSD <6.18%。所建立的UHPLC-ESI-MS / MS方法已成功用于测定来自中国不同地区的11批中华绒螯蟹样品中的核苷和核苷碱基。分析样品中总含量的范围是1329-2057μg/ g。

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