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Discovery of minor quality evaluation marker ....
Chinese patent medicines (CPMs) are popularly used in clinical practice. Though the composition is complex, the quality of CPM is usually evaluated by the contents of a few main compounds. In this study,a two-leveled metabolomics strategy was proposed to discover minor marker compounds for different CPM products. Zhenqi Fuzheng (ZQFZ) granule was studied an example, where 15 batches from 3 producers were analyzed. The samples were separated using UHPLC on an Acquity UPLC® HSS T3 column,and then detected using Q-Orbitrap-MS. In the first level, 1475 common peaks were extracted and 95 compounds were identified using diagnostic ions and a homemade database. In the second level, the data were subjected to a two-way hierarchical clustering analysis and screened by variable importance value. In total 14 marker compounds were discovered which were responsible for the grouping of different ZQFZ products. Echinacoside (22), oleoside (13), loganic acid (5), salidroside (7), ligustrosidic acid (42), 6α-hydroxygeniposide (28), and oleoside 11-methyl ester (15) could be used to reflect the quality difference for ZQFZ granule products. The proposed strategy could also contribute to the discovery of quality control markers for other CPMs.
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2. Experimental
2.1. Chemicals and reagents
The reference compounds salidroside (R1), echinacoside (R2), oleuropein (R3), specnuezhenide (R4), nuezhenoside G13 (R5), astragaloside I (R6), astragaloside III (R7), calycosin (R8) and calycosin-7-O-β-d-glucoside (R9) were purchased from Chengdu DeSiTe Biological Technology Co., Ltd. (Chengdu, China);
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An off-line three-dimensional liquid .....
ABSTRACT
To comprehensively elucidate the herbal metabolites is crucial in natural products research to discover new lead compounds. Ginsenosides are an important class of bioactive components from the Panax plants exerting the significant tonifying effects. However, to identify new ginsenosides by the conventional strategies trends to be more and more difficult because of the large spans of acid-base property(the neutral and acidic saponins), molecular mass (40 0–140 0 Da), and rather low content. Herein, an offline multidimensional chromatography/high-resolution mass spectrometry approach was presented: ion exchange chromatography (IEC) as the first dimension of separation, hydrophilic interaction chromatography (HILIC) in the second dimension, and reversed-phase chromatography (RPC) for the third dimension which was hyphenated to a Q Exactive Q-Orbitrap mass spectrometer.
By applying to the flower buds of P. ginseng (PGF), P. quinquefolius (PQF), and P. notoginseng (PNF), IEC using a PhenoSphere TM SAX column could fractionate the total extracts into the neutral (unretained) and acidic (retained) fractions, while HILIC (an XBridge Amide column) and RPC (BEH Shield RP18 column) achieved the hydrophilic interaction and hydrophobic interaction separations, respectively. Q-Orbitrap mass spectrometry offered rich structural information and complementary resolution to the co-eluting components, particular to those minor ones by including precursor ion lists in data-dependent acquisition. We could characterize 803 ginsenosides from PGF, 795 from PQF, and 833 from PNF, and 1561 thereof are potentially unknown. These results can indicate the great potential of this multidimensional approach in the ultra-deep characterization of complex herbal samples supporting the efficient discovery of potentially novel natural compounds.
Materials and methods
The reference compounds of 74 ginsenosides (Fig. S1 and Table S1) were purchased from Chengdu Desite Biotechnology Co., Ltd. (Chengdu, China).
原文链接：https://doi.org/10.1016/j.chroma.2022.463177
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细辛水提物HPLC指纹图谱及化学模式识别的研究
摘要：[目的] 通过建立中药细辛水提物高效液相色谱（HPLC）指纹图谱，评价不同产地细辛药材水提物的质量差异。[方法] 采用ZORBAX Eclipse Plus C18柱（4.6 mm×250 mm，5 μm）；以0.1%甲酸水溶液（A）-乙腈（B）为流动相进行梯度洗脱洗；流速1mL/min；柱温：30 ℃；进样量：5 μL；检测波长为285 nm。建立10 批细辛药材水提物的指纹图谱，通过相似度分析并结合聚类分析（HCA）、偏最小二乘判别分析（PLS-DA）、正交偏最小二乘法-判别分析（OPLS-DA）及主成分分析（PCA）对细辛药材水提物进行质量评价。[结果] 建立的细辛药材水提物指纹图谱共标定了20 个共有峰，通过与对照品比对，指认出6 个化学成分，10 批样品的相似度均在0.908 以上。HCA、PLS-DA、OPLS-DA 及PCA 结果表明10 批细辛药材水提物之间存在一定的质量差异，这些结果可用于对不同产地的细辛药材水提物进行质量评价。[结论] HPLC 指纹图谱结合化学模式识别技术可系统、全面地评价细辛药材水提物的质量。对中药材细辛水提物进行研究可进一步完善对细辛药材的质量评价。
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1.2试药 对照品细辛脂素（批号：DST180425-014、马兜铃酸 A （批号：DST180413-02I芝麻脂素（批号: MUST -1706301、卡枯醇（批号：DST190325-028去甲乌药碱（批号：DST190402-154、槲皮素（批号：DST180521-028购于成都德思特生物科技有限公司。
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DOI：10.11656/j.issn.1673-9043.2022.02.24
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Journal of separation science-26 November 2019
Biosurfactant trehalose lipid-enhanced ultrasound-assisted micellar extraction and determination of the main antioxidant compounds from functional plant tea期刊名：Journal of separation science文献编号：DOI 10.1002/jssc.201900910文献地址：https://onlinelibrary.wiley.com/doi/abs/10.1002/jssc.201900910发表日期：26 November 2019AbstractHydrosoluble trehalose lipid (a biosurfactant) was employed for the first time as a green extraction solution to extract the main antioxidant compounds (geniposidic acid, chlorogenic acid, caffeic acid, and rutin) from functional plant tea (Eucommia ulmoides leaves). Single‐factor tests and response surface methodology were employed to optimize the extraction conditions for ultrasound‐assisted micellar extraction combined with ultra‐high‐performance liquid chromatography in succession. A Box‐Behnken design (three‐level, three‐factorial) was used to determine the effects of extraction solvent concentration (1–5 mg/mL), extraction solvent volume (5–15 mL), and extraction time (20–40 min) at a uniform ultrasonic power and temperature. In consequence, the best analyte extraction yields could be attained when the trehalose lipid solution concentration was prepared at 3 mg/mL, the trehalose lipid solution volume was 10 mL and the extraction time was set to 35 min. In addition, the recoveries of the antioxidants from Eucommia ulmoides leaves analyzed by this analytical method ranged from 98.2 to 102%. These results indicated that biosurfactant‐enhanced ultrasound‐assisted micellar extraction coupled with a simple ultra‐high‐performance liquid chromatography method could be effectively applied in the extraction and analysis of antioxidants from Eucommia ulmoides leaf samplesStandard substances（Figure S2 in Supplementary Material）, including geniposidic acid, chlorogenic acid, caffeic acid and rutin, were obtained from Chengdu Desite Biological Technology Co., Ltd. (Chengdu,China)
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Royal society of chemistry-12 Mar 2020
The development and validation of an HPLC-MS/MS method for the determination of eriocitrin in rat plasma and its application to a pharmacokinetic study
期刊名：RSC Advances文献编号：DOI 10.1039/C9RA10925K文献地址：https://pubs.rsc.org/en/content/articlelanding/2020/RA/C9RA10925K#!divAbstract发表日期：12 Mar 2020
Abstract
Eriocitrin is one of the major active constituents of lemon fruit, and it possesses strong antioxidant, lipid-lowering, anticancer and anti-inflammatory activities and has long been used in food, beverages and wine. In this study, for the first time, a rapid, selective, and sensitive liquid chromatography-tandem mass spectrometry method (LC/MS/MS) with protein precipitation was developed and validated for the analysis of eriocitrin in rat plasma. Chromatographic separation was achieved using a mobile phase, comprising 0.1% formic acid aqueous solution and acetonitrile eluted at a flow rate of 0.8 mL min−1. In multiple reaction monitoring (MRM) modes, eriocitrin and internal standard (IS) were quantified using precursor-to-product ion transitions of m/z 595.4 → 287.1 and m/z 252.0 → 155.9, respectively. The intra- and inter-day precision (RSD) were below 6.79% in plasma, while accuracy (RE) was within ±7.67%. The matrix effect, recovery and stability were also demonstrated to be within acceptable limits. This method was successfully employed in the pharmacokinetic study on rats after the oral administration of eriocitrin. The pharmacokinetic parameters show that the maximum plasma concentration (Cmax) of eriocitrin was 299.833 ± 16.743 μg L−1, while the corresponding time to reach Cmax(Tmax) was 0.094 ± 0.019 h, and the half-time (T1/2) was 1.752 ± 0.323 h. The present results would be valuable for further research and development of eriocitrin.Eriocitrin (13463-28-0, purity > 98.5%) was obtained from Chengdu Desite Biological Technology Co., Ltd (Chengdu, China)
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