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UPLC-MS/MS法同时测定垂盆草总黄酮中8种成分的含量

王雪 蒋志涛 严国俊 邵珠莹 冯星月 潘金火

中国药房2018,Vol.29Issue(9):1222-1226,5.
中国药房2018,Vol.29Issue(9):1222-1226,5.DOI:10.6039/j.issn.1001-0408.2018.09.17

UPLC-MS/MS法同时测定垂盆草总黄酮中8种成分的含量

Simultaneous Determination of 8 Components in Total Flavanones of Sedum sarmentosum Bunge by UPLC-MS/MS

王雪 1蒋志涛 2严国俊 1邵珠莹 1冯星月 1潘金火2

作者信息

  • 1. 南京中医药大学药学院,南京210023
  • 2. 南京中医药大学附属张家港医院/江苏省企业研究生工作站,江苏张家港215600
  • 折叠

摘要

Abstract

OBJECTIVE:To establish a method for simultaneous determination of hyperoside,quercitrin,luteoloside, kaempferol,quercetin,rutin,luteolin and isorhamnetin in total flavanones of Sedum sarmentosum Bunge. METHODS:UPLC-MS/MS method was adopted. The determination was performed on ZOBAX SB C18column with mobile phase consisted of methanol-5 mmol/L ammonium formate aqueous solution(45:55,V/V)at the flow rate of 0.4 mL/min. The column temperature was 30 ℃, and sample size was 2 μL. The electrospray ionization source(ESI)was used;ion source temperature was 400 ℃;desolvation temperature was 300 ℃;desolvation gas flow was 600 L/h;capillary voltage was 3 000 V;nebuliser pressure was 45 psi;the work mode was multiple reaction monitoring mode;detection mode was negative ion mode. The established method was used to determine the contents of 8 components in 3 batches of total flavanones of Sedum sarmentosum Bunge. RESULTS:The linear ranges of hyperoside,quercitrin,luteoloside,kaempferol,quercetin,rutin,luteolin and isorhamnetin were 10.0-640.0,0.5-32.0, 4.5-288.0,8.0-512.0,50.0-3 200.0,2.0-128.0,12.5-800.0 and 25.2-1 612.8 ng/mL(r≥0.991 4),respectively. The limits of detection were 5.0,0.25,2.25,4.0,25.0,1.0,6.25 and 12.6 ng/mL,respectively.The limits of quantitation were 10.0,0.5,4.5, 8.0,50.0,2.0,12.5 and 25.2 ng/mL,separately. RSDs of precision,stability(24 h)and reproducibility tests were no more than 4.3%(n=6). The recoveries were 95.9%-100.6%,and RSDs were 1.5%-3.8%(n=6). The contents of hyperoside,quercitrin, luteoloside,kaempferol,quercetin,rutin,luteolin and isorhamnetin in 3 batches of total flavanones of Sedum sarmentosum Bunge were 507.88-560.37,42.95-50.36,63.52-71.80,1 695.10-1 753.27,10 569.28-10 612.99,25.76-30.13,2 795.22-2 877.43 and 4 869.55-4 971.30 μg/g,respectively. CONCLUSIONS:The established method can be used for simultaneous determination of 8 components in total flavanones of Sedum sarmentosum Bunge.

关键词

垂盆草/总黄酮/超高效液相色谱-串联质谱法/含量测定

Key words

Sedum sarmentosum Bunge/Total flavanones/UPLC-MS/MS/Content determination

分类

医药卫生

引用本文复制引用

王雪,蒋志涛,严国俊,邵珠莹,冯星月,潘金火..UPLC-MS/MS法同时测定垂盆草总黄酮中8种成分的含量[J].中国药房,2018,29(9):1222-1226,5.

基金项目

苏州市科技计划项目(No.SYSD2017161) (No.SYSD2017161)

中国药房

OA北大核心CSTPCD

1001-0408

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