Strategies of mobile phase transfer from thin-layer to medium-pressure liquid chromatography with silica is the stationary phase

Nyiredy, Szabolcs; Dallenbach-Toelke, K.; Zogg, G.; Sticher, Otto

doi:10.1016/s0021-9673(00)96991-7

Cited by 25 publications

(9 citation statements)

References 9 publications

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“…In this study, we report on the development of an RP-HPLC method for analyzing 19 (14), aloe-emodin (15), rhein (16), emodin (17), chrysophanol (18), and physcion (19); two di-anthrone-glucosides, sennoside B (8) and sennoside A (9) …”

Section: Electrospray Mass Spectrometric Detection (Esi-ms) Is a Somentioning

confidence: 99%

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Determination of 19 rhubarb constituents by high‐performance liquid chromatography–ultraviolet–mass spectrometry

Lin¹,

Wu²,

Lin³

et al. 2006

J of Separation Science

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Rhubarb (Rhei rhizoma), a commonly used Chinese herb, contains anthraquinones, anthrones, galloylglucoses, stilbenes, and flavan-3-ols compounds, etc. as major constituents. Using 19 of these compounds as markers, an HPLC-UV-MS method was developed to estimate the quality of rhubarb samples within a period of 70 min. Extracts were analyzed with a Cosmosil 5C18-MS column and eluted with a gradient comprising an aqueous solution of acetic acid and methanol at a flow rate of 0.9 mL/min. Peaks were detected by absorbance measurements at 254 nm (6 and 8-19) and 280 nm (1-5 and 7), and the peaks of the marker substances were identified from their UV spectra and MS fragmentation patterns. The proposed method yielded a peak-area ratio RSD value with an intraday SD falling within 0.71-1.78% and an interday SD within 0.78-1.98% at a detection limit of 0.2-3.2 microg/mL. The ESI negative ion mode was used to collect data (molecular weight, CID fragments from MS and MS/MS spectra) for 19 compounds from four types of structure categories: anthraquinones, dianthrone glycosides, stilbenes, and galloylglucosides. The information gathered can be used to identify the structures of various peaks appearing in the LC chromatograms of rhubarb samples.

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Section: Electrospray Mass Spectrometric Detection (Esi-ms) Is a Somentioning

confidence: 99%

“…Several methods have been reported for the determination of some of these rhubarb components including TLC [13][14][15], HPLC [16][17][18][19][20][21][22][23][24][25], and CE [25][26][27][28]…”

Section: Introductionmentioning

confidence: 99%

Determination of 19 rhubarb constituents by high‐performance liquid chromatography–ultraviolet–mass spectrometry

Lin¹,

Wu²,

Lin³

et al. 2006

J of Separation Science

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“…10 High-performance liquid chromatography (HPLC) for determination of five free anthraquinones is frequently used for quality control of Radix et Rhizoma Rhei according to the Chinese Pharmacopoeia and related literatures. 1,9,[11][12][13][14][15][16][17][18][19] Moreover, thin-layer chromatography (TLC), 20,21 capillary electrophoresis (CE), 22,23 ultra-performance liquid chromatography (UPLC), 6,24 UPLC-mass spectrometry (MS), 3 and high speed counter current chromatography (HSCCC) 25 also have been reported for determination of the main bioactive components in Radix et Rhizoma Rhei. However, all the analytical methods above for determining and quantifying Radix et Rhizoma Rhei suffer from the intrinsic limitations of chromatography-based methods, namely, the need of standard compounds for analyte identification or quantification and the relatively long analysis times.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous, Simple and Rapid Determination of Five Bioactive Free Anthraquinones in Radix et Rhizoma Rhei by Quantitative¹H NMR

Dong¹,

Cai²,

Fang³

et al. 2016

Journal of the Brazilian Chemical Society

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Radix et Rhizoma Rhei has been recognized for centuries in traditional medicine for its multiple pharmacological actions. The free anthraquinones including physcion, chrysophanol, emodin, rhein, and aloe-emodin are the main bioactive components in Radix et Rhizoma Rhei. In the present study, a fast quantitative 1 H nuclear magnetic resonance (q-HNMR) method for the determination and quantitation of five free anthraquinones in Radix et Rhizoma Rhei was developed. Validation of the quantitative method was performed in terms of specificity, accuracy, precision, and stability. The results showed that the solvent acetone-d 6 enabled satisfactory separation of the signals to be integrated. Five anthraquinones in Radix et Rhizoma Rhei could be quantified accurately using featured signals from 1 H NMR. This work implied that q-HNMR represents a feasible alternative to high-performance liquid chromatography (HPLC)-based methods for quantitation of anthraquinones in Radix et Rhizoma Rhei and is suitable for the quality control of Radix et Rhizoma Rhei.

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“…At present, several methods have been reported for the determination of some of these anthraquinones, including TLC [3,4], RP HPLC [5][6][7], microemulsion EKC [8], MEKC [9,10], CZE [11], cyclodextrin-modified CZE [12], and CEC [13]. However, few of these methods are entirely adequate because of poor accuracy, low resolution, or the requirement of tedious pretreatment.…”

Section: Introductionmentioning

confidence: 99%

“…Although CE has the advantages of high-resolution capability and small Figure 1. Structures of aloe-emodin (1), emodin (2), chrysophanol (3), and physcion (4). sample volume, the injection methods for sample introduction (hydrodynamic and electrokinetic sample introduction) are discontinuous in nature, and the sample throughput and precision are limited.…”

Section: Introductionmentioning

confidence: 99%

Separation and determination of four active anthraquinones in Chinese herbal preparations by flow injection-capillary electrophoresis

Fan

Chen

et al. 2005

Electrophoresis

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A simple, rapid, and accurate method for the separation and determination of physcion, chrysophanol, aloe-emodin, and emodin in Rhubarb, Juemingzi, and Chinese herbal preparations was developed by combination of flow injection-capillary zone electrophoresis for the first time. The analysis was carried out using an unmodified fused-silica capillary (75 mm x 50 microm ID x 375 microm OD, effective separation length of 48 mm) and direct ultraviolet detection at 254 nm. By a series of optimization, the sample solvent consisted of NaOH (100 mmol/L) and ACN (1:1 v/v), and a running buffer composed of 15 mmol/L sodium borate - 12.5 mmol/L sodium dihydrogen phosphate - 42% v/v ACN (pH 10.1) was applied for the separation of the four anthraquinones. The separation was rapid and highly reproducible, with complete resolution of all four compounds within 6 min. The sample throughput rate could reach up to 12 per h. The repeatability (defined as relative standard deviation) was 4.45, 4.44, 4.34, 0.61% with peak height evaluation and 1.62, 0.89, 2.49, 2.19% with peak area evaluation for physcion, chrysophanol, aloe-emodin, and emodin, respectively.

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Strategies of mobile phase transfer from thin-layer to medium-pressure liquid chromatography with silica is the stationary phase

Cited by 25 publications

References 9 publications

Determination of 19 rhubarb constituents by high‐performance liquid chromatography–ultraviolet–mass spectrometry

Determination of 19 rhubarb constituents by high‐performance liquid chromatography–ultraviolet–mass spectrometry

Simultaneous, Simple and Rapid Determination of Five Bioactive Free Anthraquinones in Radix et Rhizoma Rhei by Quantitative¹H NMR

Separation and determination of four active anthraquinones in Chinese herbal preparations by flow injection-capillary electrophoresis

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Strategies of mobile phase transfer from thin-layer to medium-pressure liquid chromatography with silica is the stationary phase

Cited by 25 publications

References 9 publications

Determination of 19 rhubarb constituents by high‐performance liquid chromatography–ultraviolet–mass spectrometry

Determination of 19 rhubarb constituents by high‐performance liquid chromatography–ultraviolet–mass spectrometry

Simultaneous, Simple and Rapid Determination of Five Bioactive Free Anthraquinones in Radix et Rhizoma Rhei by Quantitative1H NMR

Separation and determination of four active anthraquinones in Chinese herbal preparations by flow injection-capillary electrophoresis

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Simultaneous, Simple and Rapid Determination of Five Bioactive Free Anthraquinones in Radix et Rhizoma Rhei by Quantitative¹H NMR