UPLC-MS/MS同时测定山药饮片中6个核苷类成分的含量  

Simultaneous determination of 6 nucleosides in dioscoreae rhizoma decoction pieces by UPLC-MS/MS

作　　者：杨秋红 张红伟 张振凌 苏潇[1] 陈茂钦 樊磊磊 王雪芹[1] YANG Qiu-hong;ZHANG Hong-wei;ZHANG Zhen-ling;SU Xiao;CHEN Mao-qin;FAN Leilei;WANG Xue-qin(Henan Institute for Food and Drug Control,Zhengzhou 450018;State Drug Administration Key Laboratory for Quality Control of Traditional Chinese Medicine and Decoction Pieces,Zhengzhou 450018;Henan University of Chinese Medicine,Zhengzhou 450046)

机构地区：[1]河南省食品药品检验所,郑州450018 [2]国家药品监督管理局中药材及饮片质量控制重点实验室,郑州450018 [3]河南中医药大学,郑州450046

出　　处：《中南药学》2020年第5期849-853,共5页Central South Pharmacy

基　　金：2018年国家药品抽检计划中药饮片专项(食药监药化监[2017]131号):国家中药标准化建设项目(No.ZYBZH-Y-HEN-18)。

摘　　要：目的建立超高效液相色谱-三重四级杆串联质谱法(UPLC-MS/MS)同时测定山药饮片中腺嘌呤、尿嘧啶、尿苷、腺苷、肌苷、鸟苷6个核苷的含量,比较不同规格山药饮片中核苷类成分含量。方法采用ACQUITY UPLC BEH C18(2.1 mm×50 mm,1.7μm)色谱柱,以0.1%甲酸溶液-甲醇为流动相梯度洗脱,流速0.35 mL·min^-1,柱温30℃,正离子模式下多反应监测测定。结果6个核苷类成分在对应线性范围与峰面积具有良好的线性关系(R2≥0.9987),方法精密度、重复性和稳定性的RSD值均小于3.0%,平均加样回收率在97.9%~100.4%,RSD在0.98%~2.4%。不同规格山药饮片中6个核苷类成分含量有差异,山药片的核苷类成分含量显著高于山药及麸炒山药。结论该方法适用于同时测定山药饮片中6个核苷类成分含量,可用于山药饮片的质量控制。建议采用趁鲜切制等新技术加工山药,提高山药的质量。Objective To establish an UPLC-MS/MS method for the simultaneous determination of 6 nucleosides in dioscoreae rhizoma decoction pieces,and to compare the content of different specifications on nucleosides in dioscoreae rhizoma decoction pieces.Methods ACQUITY UPLC BEH C18 column(2.1 mm×50 mm,1.7μm)with gradient elution of 0.1%formic acid and methanol were adopted.The flow rate was 0.35 mL·min^-1 and the column temperature was 30℃.The target compouds were detected by positive electrospray ionization mode and multiple reaction monitoring.Results All 6 nucleosides showed good linearity(R2≥0.9987).The RSD of the precision,repeatability,and stability tests were less than 3.0%.The average recovery rates were at 97.9%-100.4%,and RSD were at 0.98%-2.4%.There was difference in content from different specifications.The content of decoction piece slices was significantly higher than decoction pieces and the processing of prepared slices of decoction pieces.Conclusion The method can simultaneously determinate 6 nucleosides and qualitativly and quantitativly analyze nucleosides in dioscoreae rhizoma decoction pieces.New technologies such as fresh slicing are encouraged to process dioscoreae rhizoma to improve its quality.

关 键 词：山药饮片 UPLC-MS/MS 腺嘌呤 尿嘧啶 尿苷 腺苷 肌苷 鸟苷 含量测定 

分 类 号：R917[医药卫生—药物分析学] R284[医药卫生—药学]