Development and Validation of a Sensitive Method for Analysis of Ellagic Acid in Dietary Supplements from Punica granatum

2020 ◽  
Vol 19 (1) ◽  
pp. 90-105
Author(s):  
Aboli Girme ◽  
Ganesh Saste ◽  
Sandeep Pawar ◽  
Chetana Ghule ◽  
Amit Mirgal ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Dietary Supplements ◽  
Ellagic Acid ◽  
Punica Granatum ◽  
Array Detector ◽  
Commercial Products ◽  
Photodiode Array Detector ◽  
Liquid Chromatography Tandem Mass ◽  
Fast Liquid Chromatography ◽  
Development And Validation

Ellagic acid is a popular antioxidant dietary supplement. It is a natural phenolic compound common to multiple botanical sources. The ellagic acid based dietary supplements are manufactured by hydrolysis of ellagitannins from Punica granatum. However, use of ellagic acid from sources other than P. granatum is not uncommon. Currently, there is no robust analytical methodologies for quantification and confirmation of the enriched ellagic acid (›40%) source in commercial products. Therefore, we have developed and validated ultra-fast liquid chromatography - photodiode array detector and ultra-fast liquid chromatography - tandem mass spectrometry methods for quantification and source identification of ellagic acid in commercial products. The results of the study confirm punicalin A-B, punicalagin A and B as positive markers and catechin and chebulinic acid as adulteration markers.

scholarly journals Development and validation of indocyanine green assay in human plasma using High-Performance Liquid Chromatography with PDA detector

2019 ◽  
Vol 10 (2) ◽  
pp. 1007-1012
Author(s):  
Sumith K Mathew ◽  
Blessed Winston A ◽  
Aswathy Mathew ◽  
Jeana Jacob ◽  
Ratna Prabha ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Indocyanine Green ◽  
High Performance ◽  
Array Detector ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Blood Specimens ◽  
Development And Validation

A robust and economical assay for routine determination of indocyanine green pharmacokinetics was developed and validated using high-performance liquid chromatography with a photodiode array detector. Plasma specimens from critically ill patients and those with hepatitis on various co-medications were used as blanks for validation of this assay. Extraction of indocyanine green was performed by simple protein precipitation with acetonitrile, and the supernatant was separated using an octadecyl column with detection at 784 nm. Blanks were found to have no interference for 40 blanks of patients who were on 56 different medications. The precision for LLOQ (0.5 µg/ml) as determined by the percentage coefficient of variation was 1.19. Stability of plasma calibration standards and stock were determined over a period of 61 days, and ICG was found to be stable for 20 days. Stability of whole blood specimens containing ICG was determined at 4°C for a period of 4 hours.

Profiling and Quantification of the Key Phytochemicals from the Drumstick Tree (Moringa oleifera) and Dietary Supplements by UHPLC-PDA-MS

Planta Medica ◽  
2020 ◽  
Author(s):  
Omer I. Fantoukh ◽  
Yan-Hong Wang ◽  
Abidah Parveen ◽  
Mohammed F. Hawwal ◽  
Gadah A. Al-Hamoud ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Dietary Supplements ◽  
High Performance ◽  
Moringa Oleifera ◽  
Negative Ion ◽  
Array Detector ◽  
Ionization Mass ◽  
Fractionation Process ◽  
Chromatography Method ◽  
Drumstick Tree

Abstract Moringa oleifera is known as a drumstick tree and is cultivated in the subtropics and tropics. It exhibits antihypertensive and antidiabetic effects. An ultra-high-performance liquid chromatography method was developed for the determination of 9 phytochemicals in M. oleifera leaves and marketed products. The efficient separation was achieved within 7 min with a temperature of 45 °C by using a C-18 column as the stationary phase and water/acetonitrile with 0.05% formic acid as the mobile phase. The method was validated for linearity, repeatability, limits of detection, and limits of quantification. The limits of detections of phenolic compounds 1 – 9 were as low as 0.2 µg/mL. The photodiode array detector at 220 and 255 nm wavelengths was recruited for quantification. The key phytochemicals were detected in the range of 0.42 to 2.57 mg/100 mg sample weight in 13 dietary supplements. This study considers the quantitative analysis for lignans in M. oleifera for the first time. Isoquercitrin (5) and quercetin 3-O-(6-O-malonyl)-β−D-glucopyranoside (6) predominates the leaves of M. oleifera with inherent degradable nature detected for compound 6. Niazirin (2) was detected in amounts between 0.010 – 0.049 mg/100 mg while compound 1 was undetectable and potentially an artifact because of the fractionation process. The characterization and confirmation of components were achieved by liquid chromatography-electrospray ionization-mass spectrometry with extractive ion monitoring for the positive and negative ion modes. The developed and validated method is robust and rapid in the conclusive quantification of phytochemicals and authentication of the Moringa samples for quality assurance.

Development and Validation of an HPLC Method for Determination of Spirotetramat and Spirotetramat cis enol in Various Vegetables and Soil

2013 ◽  
Vol 96 (3) ◽  
pp. 670-675 ◽  
Author(s):  
Balwinder Singh ◽  
Kousik Mandal ◽  
Sanjay K Sahoo ◽  
Urvashi Bhardwaj ◽  
Raminderjit Singh Battu
Keyword(s):  
Analytical Method ◽  
Anhydrous Sodium Sulfate ◽  
Hplc Method ◽  
Array Detector ◽  
Photodiode Array Detector ◽  
Photodiode Array ◽  
Precision And Accuracy ◽  
Hplc Grade Acetonitrile ◽  
Development And Validation

Abstract An easy and simple analytical method was standardized and validated for the estimation of residues of spirotetramat and its metabolite spirotetramat cis enol in various substrates: okra fruits, brinjal leaves and fruits, green chili, red chili, and soil. The samples were extracted with acetonitrile, diluted with brine solution, partitioned into dichloromethane, dried over anhydrous sodium sulfate, and cleaned up by treatment with activated charcoal powder. Final clear extracts were concentrated under vacuum and reconstituted with HPLC grade acetonitrile. Residues were estimated using HPLC with a photodiode array detector and a C18 column, and confirmed by HPTLC. Acetonitrile was used as the mobile phase at 0.4 mL/min. Both spirotetramat and spirotetramat cis enol presented distinct peak at retention times of 8.518 and 7.598 min, respectively. Consistent recoveries ranging from 82 to 97% for spirotetramat and spirotetramat cis enol were observed when samples were spiked at 1.00 to 0.03 mg/kg levels. The LOQ of the method was found to be 0.03 mg/kg. The analytical method was validated in terms of parameters, including selectivity, linearity, precision, and accuracy.

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