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印度喜马拉雅地区岩白菜属植物中的主要生物活性酚类物质:采用超高效液相色谱-四极杆/线性离子阱质谱联用技术的方法开发、验证及定量测定

Major bioactive phenolics in Bergenia species from the Indian Himalayan region: Method development, validation and quantitative estimation using UHPLC-QqQLIT-MS/MS.

作者信息

Pandey Renu, Kumar Brijesh, Meena Baleshwar, Srivastava Mukesh, Mishra Tripti, Tiwari Vandana, Pal Mahesh, Nair Narayanan K, Upreti Dalip K, Rana Tikam Singh

机构信息

Sophisticated Analytical Instrument Facility, CSIR-Central Drug Research Institute, Lucknow, India.

Academy of Scientific and Innovative Research (AcSIR), New Delhi, India.

出版信息

PLoS One. 2017 Jul 27;12(7):e0180950. doi: 10.1371/journal.pone.0180950. eCollection 2017.

DOI:10.1371/journal.pone.0180950
PMID:28749965
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC5531703/
Abstract

Bergenia species are important medicinal plants used in indigenous systems of medicine for their antilithiatic and diuretic properties. An ultra-high performance liquid chromatography coupled to hybrid linear ion trap triple quadrupole mass spectrometry (UHPLC-QqQLIT-MS/MS) method has been developed and validated for the estimation of quantitative variation of eight major bioactive phenolics in the rhizomes (150 samples) of four species of this herb, Bergenia (B. ciliata, B. ligulata, B. purpurascens and B. stracheyi). Chromatographic separation was obtained on a Waters ACQUITY UPLCTM BEH (ethylene bridged hybrid) C18 column with a mobile phase consisting of 0.1% (v/v) formic acid aqueous solution and acetonitrile under a gradient elution manner. A hybrid linear ion trap triple quadrupole mass spectrometer was operated in negative electrospray ionization mode with multiple reactions monitoring for detection and quantification of the eight compounds. The validated method demonstrated good linearity (r2 ≥ 0.9991), precision (RSD ≤ 1.87%) and accuracy (95.16-102.11%, RSD ≤ 1.83%) for all reference analytes. The quantitative results revealed that B. ligulata contains the highest amount of the major active marker-bergenin. The results also suggest that sensitive UHPLC-QqQLIT-MS/MS method, a sensitive, accurate and convenient one, could be helpful in identification of potential accession(s), rapid quality control and establishing authenticity of Bergenia species as raw material for pharmaceutical industries.

摘要

岩白菜属植物是重要的药用植物,在传统医学体系中因其抗结石和利尿特性而被使用。已开发并验证了一种超高效液相色谱-混合线性离子阱三重四极杆质谱联用(UHPLC-QqQLIT-MS/MS)方法,用于测定该草药四种岩白菜属植物(岩白菜、光叶岩白菜、紫花岩白菜和长梗岩白菜)根茎(150个样品)中八种主要生物活性酚类的定量变化。在沃特世ACQUITY UPLCTM BEH(乙烯桥接杂化)C18柱上进行色谱分离,流动相由0.1%(v/v)甲酸水溶液和乙腈组成,采用梯度洗脱方式。混合线性离子阱三重四极杆质谱仪在负电喷雾电离模式下运行,通过多反应监测对八种化合物进行检测和定量。验证后的方法对所有参考分析物均显示出良好的线性(r2≥0.9991)、精密度(RSD≤1.87%)和准确度(95.16 - 102.11%,RSD≤1.83%)。定量结果表明,光叶岩白菜中主要活性标志物岩白菜素的含量最高。结果还表明,灵敏的UHPLC-QqQLIT-MS/MS方法灵敏、准确且方便,有助于鉴定潜在种质、快速质量控制以及确定岩白菜属植物作为制药行业原材料的真实性。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/4f0c/5531703/9f632edc5d31/pone.0180950.g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/4f0c/5531703/b74e9e523f7c/pone.0180950.g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/4f0c/5531703/7142c9fe8525/pone.0180950.g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/4f0c/5531703/9f632edc5d31/pone.0180950.g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/4f0c/5531703/b74e9e523f7c/pone.0180950.g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/4f0c/5531703/7142c9fe8525/pone.0180950.g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/4f0c/5531703/9f632edc5d31/pone.0180950.g003.jpg

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