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高粱泡叶中异槲皮素TLC鉴别与HPLC含量测定研究
摘要：目的 通过建立高粱泡叶药材中异槲皮素活性成分的薄层鉴别(TLC)及高效液相色谱分析方法(HPLC)测定槲皮素含量。方法 70%乙醇为溶剂超声提取高粱泡叶中异槲皮素,以乙酸乙酯∶甲酸∶水∶氨水(18∶2∶1∶0.5)为展开剂于聚酰胺薄膜上展开,3%三氯化铝乙醇溶液为显色剂,105℃烘3 min, 365 nm下检视。采用HPLC,以异槲皮素为对照品,色谱柱为Agilent SB-C18柱(5μm, 4.6 mm×150 mm),以乙腈为流动相(B),以水(含2%磷酸)为流动相(A),梯度洗脱,洗脱程序如下:0~2 min, 10.0%~15.0%B;2~22 min, 15.0%~19.5%B;22~26 min, 19.5%~21.0%B;26~30 min, 21.0%~20.0%B;30~35 min, 20.0%~10.0%B;35~45 min, 10.0%B。柱温30℃,检测波长360 nm,流速1.0 mL/min。结果 高粱泡叶中异槲皮素在紫外灯下出现明显斑点。异槲皮素2~20μL范围内呈良好的线性关系,相关系数(r)为1,平均回收率(n=9)分别为95%,99%,103%,RSD分别为1.0%,0.8%,0.6%。结论 本实验所建立的高梁泡叶药材异槲皮素含量测定方法简便快速、准确可行,通过对高粱泡叶薄层色谱及含量测定方法的建立,为后期高粱泡叶的应用开发奠定相关基础。
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药品与试剂 异槲皮素对照品（批号：DST-DT000601，供含量测定用，乐美天医药德思特生物）；
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Journal of separation science-03 March 2019
Ionic liquid vortex-simplified matrix solid-phase dispersion for the simultaneous determination of terpenoids, crocins, quinic acid derivatives and flavonoids in Gardeniae fructus by UHPLC期刊名：Journal of separation science文献编号：DOI 10.1002/jssc.201801354文献地址：https://onlinelibrary.wiley.com/doi/abs/10.1002/jssc.201801354发表日期：03 March 2019AbstractA novel ionic‐liquid‐based vortex‐simplified matrix solid‐phase dispersion method using 2,6‐dimethyl‐β‐cyclodextrin was established by ultra high performance liquid chromatography coupled with a photodiode array detector. 2,6‐Dimethyl‐β‐cyclodextrin was first used as a promising adsorbent in this proposed method for simultaneous determination of eight compounds in Gardeniae fructus. These compounds are terpenoids (geniposidic acid, genipin‐1‐β‐D‐gentiobioside, geniposide, 8‐o‐acetyl shanzhiside methyl ester), crocins (crocin‐I, crocin‐II), quinic acid derivatives (chlorogenic acid), and flavonoids (isoquercitrin), respectively. Several parameters were investigated in the adsorption and desorption processes to obtain the optimal conditions, including 2,6‐dimethyl‐β‐cyclodextrin as sorbent, 0.5 mL 100 mM 1‐dodecyl‐3‐methylimidazolium hydrogen sulfate as the extraction solvent, 2:1 of sample/sorbent ratio, grinding for 2 min and vortexing for 60 s. The recoveries of the eight compounds ranged from 96.6 to 100% (<3.50%). The limits of detection and quantification were in the range of 0.02–0.30 and 0.06–1.25 μg/mL, respectively. Meanwhile, a good linearity was attained with r values (>0.9997). The established method showed higher extraction efficiency and less reagent consumption than traditional matrix solid phase dispersion and ultrasonic‐assisted extraction. Hence, it could be applied for sample preparation and analysis of natural products.Standard substances including geniposidic acid, chlorogenic acid, genipin-1-β-Dgentiobioside, geniposide, 8-o-acetyshanzhiside methyl ester, isoquercitrin, crocin I, and crocin II were purchased from Chengdu Desite Biological Technology Co., Ltd(Chengdu, China).
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Frontiers in pharmacology-09 January 2019
Simultaneous Extraction and Determination of Compounds With Different Polarities From Platycladi Cacumen by AQ C18-Based Vortex-Homogenized Matrix Solid-Phase Dispersion With Ionic Liquid期刊名：Frontiers in pharmacology文献编号：DOI 10.3389/fphar.2018.01532文献地址：https://link.springer.com/article/10.1007%2Fs13318-017-0444-8发表日期：09 January 2019 This study presented a rapid, simple and environmentally friendly method of employing AQ C18-based vortex-homogenized matrix solid-phase dispersion with ionic liquid (AQ C18-IL-VHMSPD) for the extraction of compounds with different polarities from Platycladi Cacumen (PC) samples by ultra high-performance liquid chromatography with PDA detection. AQ C18 (aqua C18) and ionic liquid ([Bmim]BF4) were used as the adsorbent and green elution reagent in vortex-homogenized MSPD procedure. The AQ C18-IL-VHMSPD conditions were optimized by studying several experimental parameters including the type of ionic liquid, the type of adsorbent, ratio of sample to adsorbent, the concentration and volume of ionic liquid, grinding time and vortex time. The recoveries of the target compounds were in the range of 96.9–104% with relative standard deviation values no more than 2.8%. The limits of detection and limits of quantitation were in the range of 0.2–1.2 and 1.0–5.4 ng mL-1, respectively. Compared with the traditional ultrasonic-assisted extraction, the developed AQ C18-IL-VHMSPD method required less sample, reagent and time. It was concluded that the AQ C18-IL-VHMSPD method was a powerful method for the extraction and quantification of the high polarity and low polarity compounds in traditional Chinese medicines samples.Reference standards of myricitrin, isoquercitrin, quercitrin,amentoflavone and hinokiflavone were purchased from Chengdu Desite Biological Technology Co., Ltd (Chengdu, China)
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Pharmacokinetic comparison of fifteen active compositions in rat plasma after oral administration of raw and honey-processed Aster tataricus extracts
A sensitive ultra-high performance liquid chromatography–tandem mass spectrometry method was developed and validated to clarify pharmacokinetic properties of 15 compounds (quercetin, isorhamnetin, chlorogenic acid, isoquercitrin, caffeic acid, scopoletin, 7-hydroxycoumarin, shionone,ferulic acid, kaempferol-7-O-β-D-glucopyranoside, methyl caffeate, luteolin, kaempferol,epifriedelinol, and protocatechuic acid) in raw and honey-processed Aster tataricus. Separation was carried out on an ACQUITY UPLC® BEH C18 column (2.1 × 100 mm, 1.7 µm) using a gradient elution with mobile phase constituting 0.1% formic acid-water and 0.05% formic acid-methanol.Quantitative analysis was performed using multiple reaction monitoring detection in both positive and negative ionization modes. Calibration curves showed good linearity (r2 > 0.991) over the corresponding concentration range. The intra-day and inter-day precisions were within 10.1%, and accuracy ranged from -11.4% to 12.4%. The extraction recoveries and matrix effects were 78.1%–100.0% and 81.1%–113.7%, respectively. The analytes were stable under four storage conditions with relative standard deviations less than 12.6%. The validated method was successfully applied to compare the pharmacokinetic behaviors of raw and honey-processed Aster tataricus for the first time. The results indicated that the AUCs of shionone, ferulic acid, and protocatechuic acid in honey-processed Aster tataricus group were significantly lower than that of raw Aster tataricus group.
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Standards, including quercetin, isorhamnetin, scopoletin, 7-hydroxycoumarin, shionone, kaempferol-7-O-β-D-glucopyranoside, methyl caffeate, luteolin, kaempferol, protocatechuic acid,
and icariin (internal standard, IS) (purity ≥ 98%) were purchased from Chengdu Desite
Bio-Technology Co., Ltd. (Chengdu, China).
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Comprehensive evaluation of the antioxidant capacity of Sceptridium ternatum using multiple colorimetric methods and 1,1‐diphenyl‐2‐picrylhydrazyl–high‐performance liquid chromatography analysis
Sceptridium ternatum is a medicinal herb with multiple health benefits. However, its antioxidant activity and active components have not been clarified. In this study, the antioxidant capacity of S. ternatum was comprehensively investigated using multiple colorimetric methods and 1,1‐diphenyl‐2‐picrylhydrazyl–high‐performance liquid chromatography analysis. First, the phenolic content, flavonoid content, and radical scavenging ability of S. ternatum were parallelly determined using colorimetric methods performed in 96‐well microplates. The flavonoid content, rather than the phenolic content, was highly correlated with its antioxidant activity. Sceptridium ternatum was shown to be a rich source of flavonoids, with a highest flavonoid yield of 3.44 ± 0.11 mg/g. Subsequently, 1,1‐diphenyl‐2‐picrylhydrazyl–high‐performance liquid chromatography experiment and quadrupole time‐of‐flight mass spectrometry analyses were carried out for rapid screening of the individual antioxidants. A total of 14 O‐glycosyl flavonoids with quercetin or kaempferol aglycone have been characterized. Particularly, quercetin 3‐O‐rhamnoside‐7‐O‐glucoside exhibited the most potent antioxidant ability. Its half‐maximal effective concentrations for scavenging 1,1‐diphenyl‐2‐picrylhydrazyl and 2,2ʹ‐azino‐bis (3‐ethylbenzthiazoline‐6‐sulfonic acid) radicals were 70.55 ± 2.69 and 106.90 ± 1.76 µg/mL, respectively, which were comparable with those of l‐ascorbic acid. Our results indicated that the combined colorimetric and chromatographic methods provided a practical strategy for the discovery of bioactive compounds from natural products. ...... Quercetin (Que, ≥98% purity) was procured from Chengdu Desite Biotech (Chengdu, China).
原文链接;https://doi.org/10.1002/jssc.202000550
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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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