UFLC-QTRAP-MS/MS法测定绞股蓝中10个核苷类成分  

Determination of 10 nucleosides in Gynostemma pentaphyllum by UFLC-QTRAP-MS/MS

作　　者：马赟[1] 蔡静[1] 张园娇 纪乐军 陈建伟[1] 李祥[1] 

机构地区：[1]南京中医药大学药学院,南京210023 [2]江苏神华药业有限公司,淮安211600

出　　处：《药物分析杂志》2017年第12期2154-2161,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：江苏省科技成果转化项目(BA2014118);江苏高校优势学科建设工程资助项目(PAPD)

摘　　要：目的:建立UFLC-QTRAP-MS/MS的方法,同时测定不同产地绞股蓝及其商品药材中10个化合物(胸苷、尿苷、腺苷、肌苷、2′-脱氧鸟苷、鸟苷、腺嘌呤、次黄嘌呤、尿嘧啶、鸟嘌呤)的含量。方法:采用XBridge Amide色谱柱(2.1 mm×100 mm,3.5μm),以0.2%甲酸水溶液(A)-0.2%甲酸乙腈溶液(B)为流动相,0.6 m L·min^(-1)流速梯度洗脱,正离子(ESI+)模式下多反应监测(MRM)检测。结果:尿嘧啶、胸苷、尿苷、次黄嘌呤、肌苷、2′-脱氧鸟苷、腺苷、鸟苷、腺嘌呤、鸟嘌呤的线性范围分别为1.97~3 936.00、2.00~200.00、30.48~3 048.00、19.84~1 984.00、10.16~1 016.00、4.95~990.00、19.72~1 972.00、14.70~2 940.00、1.96~196.00、14.76~1 476.00 ng·m L^(-1)(r>0.997 3),平均加样回收率为99.3%~101.3%,含量分别为181.54~1 604.95、0.00~216.45、63.65~1 093.17、3.48~555.12、0.07~215.66、0.00~171.65、0.00~338.63、24.67~966.08、0.37~140.07、14.89~830.79μg·g^(-1),绞股蓝中以尿嘧啶、尿苷、鸟苷、鸟嘌呤含量较高;不同产地及商品药材中10个成分含量有所差异。结论:该方法为绞股蓝药材内在质量的综合评价提供新的科学依据。Objective： To establish a method for simultaneous determination of 10 components （ thymidine, uridine, adenosine, inosine, 2＇ -deoxyguanosine, guanosine, adenine, hypoxanthine, uracil and guanine ） in Gynostemma pentaphyllum from different habitats and commercial sources by ultra-fast liquid chromatography tandem combined with triple quadrupole mass spectrometry （ UFLC-QTRAP-MS/MS ）. Methods： The analysis was carried out on an XBridge Amide column（ 2.1 mm × 100 mm, 3.5 μm ）which was eluted by a mobile phase of 0.2% formic acid - 0.2% formic acid in acetonitrile at a flow rate of 0.6 mL·min-1. The target compounds were analyzed by the positive ion multiple reaction monitoring （ MRM ） mode. Results： Uracil, thymidine, uridine, hypoxanthine, inosine, 2＇ -deoxyguanosine, adenosine, guanosine, adenine and guanine showed good linearity （ r 〉 0.997 3 ）in the range of 1.97-3 936.00 ng·mL-1, 2.00-200.00 ng·mL-1 30.48-3 048.00 ng·mL-1, 19.84-1 984.00 ng·mL-I, 10.16-1 016.00 ng·mL-1, 4.95-990.00 ng·mL-I, 19.72-1 972.00 ng·mL-1, 14.70-2 940.00 ng·mL-l, 1.96- 196.00 ng·mL-1 and 14.76-1 476.00 ng· mL-1, respectively. The average recoveries of the ten components were between 99.3% and 101.3%. The contents of ten components were in the range of 181.54-1 604.95μg·g-1, 0.00- 216.45μg·g-1, 63.65-1 093.17μg·g-1,3.48-555.12μg·g-1, 0.07-215.66μg·g-1, 0.00-171.6 5μg·g-1, 0.00-338.63μg·g-1, 24.67-966.08μg·g-1, 0.37-140.07μg·g-1, and 14.89-830,79μg·g-1, respectively. The contents of uracil, uridine, guanosine and guanine were higher in Gynostemma pentaphyllum. The contents of ten components varied by habitats and commercial sources. Conclusion： The established method provides scientific basis for the comprehensive quality evaluation of Gynostemma pentaphyllum.

关 键 词：绞股蓝 药食同源 胸苷 尿苷 腺苷 肌苷 2′-脱氧鸟苷 鸟苷 腺嘌呤 次黄嘌呤 尿嘧啶 鸟嘌呤 高分离度快速液相色谱质谱联用 

分 类 号：R917[医药卫生—药物分析学]