scholarly journals An Improved LC-MS/MS Method for Simultaneous Determination of the Eleven Bioactive Constituents for Quality Control of Radix Angelicae Pubescentis and Its Related Preparations

2015 ◽  
Vol 2015 ◽  
pp. 1-10 ◽  
Author(s):  
Jin Li ◽  
Qiu-Hong Zhang ◽  
Jun He ◽  
Er-wei Liu ◽  
Xiu-mei Gao ◽  
...  
Keyword(s):  
Quality Control ◽  
Simultaneous Determination ◽  
Control Method ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Bioactive Constituents ◽  
Linear Gradient ◽  
Radix Angelicae Pubescentis ◽  
Aqueous Ammonium Acetate

An improved LC-MS/MS method was developed for simultaneous determination of eleven bioactive constituents of Radix Angelicae Pubescentis and its related preparations. It was the first report on the quantification of bioactive constituents in different preparations of Radix Angelicae Pubescentis by LC-MS/MS analytical method. These samples were separated with an Agilent Zorbax Extend reversed-phase C18 column (1.8 μm, 4.6 × 100 mm) by linear gradient elution using aqueous ammonium acetate and acetonitrile as mobile phase. The flow rate was 0.3 mL min−1. The eleven bioactive constituents showed good regression(R>0.990)within test ranges and the recoveries were in the range of 87.1–110%. The limit of detections and quantifications for most of the major constituents were less than 0.5 and 1.0 ng mL−1, respectively. All results indicated that the developed method could be readily utilized as a suitable quality control method for Radix Angelicae Pubescentis and related preparations.

Simultaneous Determination of Eight Potential Q-Markers in Zishen Tongguan Capsules Based on UHPLC-MS/MS

2020 ◽  
Vol 17 (1) ◽  
pp. 47-56
Author(s):  
Shun Liu ◽  
Xun Wang ◽  
Kaiping Zou ◽  
Wei Liu ◽  
Cunyu Li ◽  
...  
Keyword(s):  
Quality Control ◽  
Chinese Medicine ◽  
Simultaneous Determination ◽  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Quality Markers ◽  
High Repeatability ◽  
Comprehensive Study

Background: Zishen Tongguan (ZSTG) capsules were prepared at the Affiliated Hospital of Nanjing University of Chinese Medicine and have been proven to be clinically effective for treating pyelonephritis and benign prostatic hyperplasia. However, the quality standards are not ideal; a comprehensive study of the “quality markers” (Q-markers), the chemicals inherent in traditional Chinese medicine and its preparations, has not been carried out. Experimental Methods: In this paper, a sensitive and specific ultra-high-performance liquid chromatographictandem mass spectrometry (UHPLC-MS/MS) method was developed for the simultaneous determination of eight potential Q-markers of ZSTG, including timosaponin A3, berberine, jatrorrhizine, phellodendrine, palmatine, mangiferin, neomangiferin, and timosaponin BII. A Kromasil 100-3.5 C18 column was used with a mobile phase of 0.2% formic acid with acetonitrile, and gradient elution at a flow rate of 0.2 mL/min was achieved in 13 minutes and used for separation. Detection was performed in positive/negative mode with multiple reaction monitoring (MRM). Results: The analytical method was validated in terms of the sensitivity, linearity, accuracy, precision, repeatability, stability and recovery. The method established here was successfully applied to study the potential Q-markers in 8 batches of commercial samples, which demonstrated its use in improving the quality control of ZSTG. Conclusion: The developed method had high repeatability and accuracy and was suitable for the simultaneous analysis of multiple Q-markers, which may provide a new basis for the comprehensive assessment and overall quality control of ZSTG.

scholarly journals Fast and selective HPLC-DAD method for determination of pholcodine and related substances

2011 ◽  
Vol 30 (2) ◽  
pp. 139 ◽  
Author(s):  
Ana Petkovska ◽  
Hristina Babunovska ◽  
Marina Stefova
Keyword(s):  
Quality Control ◽  
Degradation Products ◽  
Ammonium Hydroxide ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Real Sample Analysis ◽  
Related Substances ◽  
Structural Analogues ◽  
Reliable Methods

Quality control of pharmaceuticals requires development of fast, efficient and reliable methods for determination of active compounds as well as known and very often unknown impurities within defined concentration ranges. In this work, a simple and rapid HPLC-UV-DAD method for identification and quantification of pholcodine process related impurities and some degradation products was developed and validated. Pholcodine and its five structural analogues such as morphine, codeine, thebaine, oripavine, and papaverine were separated in less than 10 minutes using reversed phase LiChrospher C-8 column. For optimal chromatographic performance with reproducible retention times, gradient elution with 2% ammonium hydroxide in water and acetonitrile was used. The method was validated by establishing its selectivity, specifity, sensitivity, linearity, intra- and inter-day precision and robustness. All tested parameters confirmed that the method is suitable for determination of pholcodine and its five impurities in pharmaceutical drug samples. The results obtained from real sample analysis give support to the suitability of the proposed method for the purpose of quality control.

scholarly journals Simultaneous Determination of Four Major Constituents of Semen Vaccariae Using HPLC-DAD

2012 ◽  
Vol 7 (9) ◽  
pp. 1934578X1200700 ◽  
Author(s):  
Haijiang Zhang ◽  
Wei Yao ◽  
Yunyun Chen ◽  
Peipei He ◽  
Yao Chen ◽  
...  
Keyword(s):  
Quality Control ◽  
Quantitative Analysis ◽  
Simultaneous Determination ◽  
Chromatographic Separation ◽  
Gradient Elution ◽  
Hplc Method ◽  
Frying Temperature ◽  
Simultaneous Quantification ◽  
Frying Process

A simple and reliable HPLC method was developed and validated for the simultaneous quantification of four major constituents in Semen Vaccariae. The chromatographic separation was performed on an Agilent Zorbax SB-C18 column with gradient elution using methanol and water. The calibration curves showed good linearity of R2 > 0.9999 with LOQs (S/N = 10) of 0.20–1.16 μg/mL. The precision was evaluated by intra- and inter-day assays and R.S.D. values were less than 2.09%. The recovery rates were between 97.0% and 105.0%. The developed method was applied to the quantitative analysis of Semen Vaccariae and its stir-fried products. During the stir-frying process, vaccarin degraded and yielded isovitexin-2″- O-arabinoside. The preferable stir-frying temperature is around 120°C. The developed HPLC method can be applied to the quality control of crude and stir-fried Semen Vaccariae.

scholarly journals Simultaneous Determination of Eight Synthetic Permitted and Five Commonly Encountered Nonpermitted Food Colors in Various Food Matrixes by High-Performance Liquid Chromatography

2010 ◽  
Vol 93 (5) ◽  
pp. 1503-1514 ◽  
Author(s):  
Sumita Dixit ◽  
Subhash K Khanna ◽  
Mukul Das
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
High Sensitivity ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Hplc Method ◽  
Food Category ◽  
Food Commodities ◽  
Food Colors

Abstract A simple and sensitive HPLC method has been developed for the simultaneous determination of eight permitted food colors and five commonly encountered nonpermitted colors in various food commodities, including sugar-, fat-, and starch-based food matrixes. The method uses a specific food category-based cleanup/treatment procedure before color extraction to avoid the interference of food matrixes, and to obtain the optimal color extraction. Analysis was performed on a reversed-phase C18 -Bondapak column with ammonium acetate and acetonitrile gradient elution as the mobile phase; a programmable max-specific visible detection was used to monitor colors to obtain the higher sensitivity and expanded scope needed for multicolor blends having diverse absorption maxima. All colors showed good linearity, with regression coefficients of 0.99740.9999. The LOD and LOQ values ranged from 0.01 to 0.12 mg/L, and from 0.04 to 0.83 mg/L or mg/kg, respectively. The intraday and interday precision tests produced good RSD values, and the recoveries from different food matrixes ranged from 82 to 104%. The method offers high sensitivity for analysis of a wide variety of food matrixes containing a broad scope of multicolor blends. Two nonpermitted colors, orange II and metanil yellow, were found. Also, a number of samples contained permitted colors at levels two-to seven-fold higher than those prescribed.

Simultaneous Determination of Danshensu, Salvianolic Acid B, and Paeonol in ShuangDan Oral Liquid by HPLC

2013 ◽  
Vol 96 (1) ◽  
pp. 20-23 ◽  
Author(s):  
Hua Li ◽  
Siwang Wang ◽  
Yanhua Xie ◽  
Bangle Zhang ◽  
Jianbo Wang ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Control Method ◽  
Medicinal Preparation ◽  
Gradient Elution ◽  
Salvianolic Acid B ◽  
Array Detector ◽  
Column Temperature ◽  
Salvianolic Acid ◽  
Oral Liquid

Abstract An HPLC-photodiode array detector (PDAD) method was developed for simultaneous determination of danshensu, salvianolic acid B, and paeonol in a traditional Chinese medicinal preparation ShuangDan oral liquid, which is widely used to treat coronary heart disease in China. The samples were separated on a SinoChrom ODS–BP C18 column with the column temperature maintained at 30°C. The mobile phase was composed of methanol and 2% (v/v) glacial acetic acid at a flow rate of 1.0 mL/min. The separation was finished within 30 min using linear gradient elution. All calibration curves showed good linearity (r > 0.9997) within the test ranges. The method was simple, reliable, accurate, and specific. The intraday and interday precisions (RSD) were less than 0.85%. The recoveries were between 96.97 and 102.14%. The method was successfully applied to the determination of the three components in three commercial samples of ShuangDan oral liquid. The results indicated that the developed HPLC–PDAD assay could be readily utilized as a comprehensive quality control method for ShuangDan oral liquid.

Development of a Method for Simultaneous Determination of Two Stilbenes and Four Anthraquinones from Polygonum Cuspidatum by RP-HPLC

2019 ◽  
Vol 102 (1) ◽  
pp. 69-74 ◽  
Author(s):  
Jianye Yan ◽  
Yuanqing Wang ◽  
Hongnian Wu ◽  
Zhicheng Sun ◽  
Shihan Tan ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Polygonum Cuspidatum ◽  
Chinese Medicinal Herb ◽  
Simple Method ◽  
Rp Hplc ◽  
First Time

Abstract Background: Polygonum Cuspidatum Sieb. et Zucc. (named Huzhang in China) is a traditional and popular Chinese medicinal herb used in removing jaundice, clearing heat-toxin, improving blood circulation, expelling stasis, dispelling wind and dampness, repelling phlegm, and suppressing cough. It is widely used in drug and functional food fields and distributed throughout the world, including in China, Japan, and North America. Objective: To control the quality of Polygonum Cuspidatum, an effective, reliable, and simple method for simultaneous determination of two stilbenes (polydatin, resveratrol) and four anthraquinones (emodin, physcion, rhein, and anthraglycoside B) was developed and validated for the first time in this study by reversed-phase HPLC (RP-HPLC). Methods: Separation was carried out on Agilent C18 column (250 × 4.6 mm I.D., 5 μm) with acetonitrile and 0.10% aqueous phosphoric acid as mobile phase and gradient elution at a flow rate of 0.8 mL/min. Detection was conducted with mobile wavelength at 30°C. Results: Good validation of the method including linearity, precision, repeatability, and recovery was performed. The contents of the studied analytes are significantly different, and resveratrol and rhein in particular existed in greater fluctuation among the samples. Conclusion: A simple, reliable, and sensitive method has been successfully established and applied to the analysis for simultaneous determination of the target compounds in 11 batches of samples. Highlights: Separation and quantitative analysis of two stilbenes and four anthraquinones from P. cuspidatum were developed by RP-HPLC. This method is convenient, sensitive, and accurate and can provide a reliable basis for further applications of P. cuspidatum in drug or food fields.

scholarly journals Analysis of Flavonoids and Iridoids in Vitex Negundo by HPLC-PDA and Method Validation

2013 ◽  
Vol 8 (9) ◽  
pp. 1934578X1300800
Author(s):  
Somendu K. Roy ◽  
Khemraj Bairwa ◽  
Jagdeep Grover ◽  
Amit Srivastava ◽  
Sanjay M. Jachak
Keyword(s):  
Quality Control ◽  
Simultaneous Determination ◽  
Method Validation ◽  
Hplc Method ◽  
Vitex Negundo ◽  
Good Recovery ◽  
Bioactive Constituents ◽  
Ich Guidelines ◽  
Validation Parameters

The leaves of Vitex negundo have been reported to contain various bioactive constituents including iridoids and flavonoids. This is the first report on the simultaneous determination of iridoids and flavonoids by HPLC in three different samples of V. negundo leaves collected from three regions of India. Separation of iridoids and flavonoids was accomplished by HPLC and further elaborated for their quantification in V. negundo leaves using a C-18 column with detection at 254 and 330 nm, respectively. The developed HPLC method showed good linearity (r2≥0.999), high precision (RSD<5%) and a good recovery (99.3–103.0%) of the compounds. All the validation parameters of the developed HPLC were found to be within the permissible limits according to the ICH guidelines. The developed method was robust, accurate and reliable for the quality control of V. negundo leaves.

scholarly journals Quality Control of the Fuzi Lizhong Pill Through Simultaneous Determination of 16 Major Bioactive Constituents by RRLC–MS-MS

2018 ◽  
Vol 56 (6) ◽  
pp. 541-554 ◽  
Author(s):  
Yun-zhuo Dong ◽  
Zhen-li Liu ◽  
Yuan-yan Liu ◽  
Zhi-qian Song ◽  
Na Guo ◽  
...  
Keyword(s):  
Quality Control ◽  
Simultaneous Determination ◽  
Bioactive Constituents
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