Development and Validation of a UHPLC-PDA-MS Method for the Quantitative Analysis of Anthraquinones in Bulbine natalensis Extracts and Dietary Supplements

Planta Medica ◽  
2019 ◽  
Vol 86 (02) ◽  
pp. 144-150 ◽  
Author(s):  
Ji-Yeong Bae ◽  
Bharathi Avula ◽  
Yan-Hong Wang ◽  
Mei Wang ◽  
Zulfiqar Ali ◽  
...  

AbstractA UHPLC-photodiode array-MS method was developed and validated for the quantification of one chromone and six anthraquinone type of compounds from Bulbine natalensis plant samples and dietary supplements. Metabolites 1 –  7 were identified based on their retention times and electrospray ionization-MS spectra compared with a mix of previously isolated compounds. The quantification of 1 –  7 was based on photodiode array detection. The optimized separation was achieved using a CORTECS C18 column with a gradient of water/acetonitrile as the mobile phase. Seven compounds were separated within 15 minutes with detection limits of 50 pg on the column. The analytical method was validated for linearity, repeatability, accuracy, limits of detection, and limits of quantification. The relative standard deviations for intra- and inter-day experiments were less than 5% and the recovery efficiency was 98 – 101%. Nine dietary supplements labeled as containing B. natalensis were examined. Anthraquinone-type compounds were detected in only five out of nine dietary supplements, with the total amount ranging from 11.3 to 90.4 mg per daily dose. The analytical method is simple, economic, rapid, and can be applied for quality assessment of B. natalensis and dietary supplements. Electrospray ionization-MS was used for the identification of these compounds in plant samples and dietary products.

2011 ◽  
Vol 94 (5) ◽  
pp. 1383-1390
Author(s):  
Bharathi Avula ◽  
Yatin J Shukla ◽  
Yan-Hong Wang ◽  
Ikhlas A Khan

Abstract An HPLC method was developed for the quantitative determination of five pregnane derivatives from aerial parts of Caralluma species and dietary supplements. The method was validated for linearity, repeatability, LOD, and LOQ. The LOD and LOQ of five pregnane compounds were found to be in the range of 1–5 and 3–15 μg/mL, respectively, by HPLC using photodiode array detection. This method was applied to the identification of three plant materials of Caralluma species (C. fimbriata, C. umbellate, and C. attentuata) and seven dietary supplements claiming to contain C. fimbriata. An LC/MS coupled with electrospray ionization interface method was used for the identification of compounds and involved the use of [M+Na]+ ions in the positive ion mode with extracted ion chromatogram.


Planta Medica ◽  
2017 ◽  
Vol 84 (08) ◽  
pp. 536-543 ◽  
Author(s):  
Weize Zhang ◽  
Guo Nan ◽  
Hong-Hua Wu ◽  
Miaomiao Jiang ◽  
Tian-Xiang Li ◽  
...  

Abstract Nardostachys jatamansi is a well-documented herbal agent used to treat digestive and neuropsychiatric disorders in oriental medicinal systems. However, few simple, rapid, and comprehensive methods were reported for quality assessment and control of N. jatamansi. Herein, a UPLC with photodiode array detection method was developed for both fingerprint investigation of N. jatamansi and simultaneous quantitative analysis of the six serotonin transporter modulatory constituents in N. jatamansi. For chromatographic fingerprinting, 24 common peaks were selected as characteristic peaks to assess the consistency of N. jatamansi samples from different retail sources. Six of the common peaks (5, 7, 12, and 16 – 18) were identified as desoxo-narchinol A, buddleoside, isonardosinone, nardosinone, kanshone H, and (−)-aristolone, respectively, by phytochemical investigation. Five of the six compounds significantly either enhanced or inhibited serotonin transporter activity, while (−)-aristolone (18) didnʼt show any serotonin transporter activity. In quantitative analysis, the six compounds showed good linearity (r > 0.999) within test ranges. The precision, expressed as relative standard deviation, was in the range of 0.25 – 2.77%, and the recovery of the method was in the range of 92 – 105%. The UPLC-photodiode array detection-based fingerprint analysis and quantitative methods reported here could be used for routine quality control of N. jatamansi.


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