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A validated UHPLC-PDA with an ESI-MS/MS method has been developed for simultaneous estimation of six bioactive alkaloids (magnoflorine, berbamine, columbamine, jatrorrhizine, palmatine and berberine) in the different extracts of the roots of Berberis aristata DC (Family:Berberdiaceae). It is an important medicinal herb native to Northern Himalaya and commonly known as ‘daruharidra’, ‘daruhaldi’, ‘Indian barberry’ or ‘tree turmeric’. An insight into the research literature uncovered reports on isoquinoline alkaloids like magnoflorine, berbamine, columbamine, jatrorrhizine, palmatine, and berberine as major bioactives in B. aristata roots, possessing different pharmacological and therapeutic effects. In the present study, these aforementioned alkaloids were separated on Phenomenex Luna®, 5 µm-C8 analytical column. The HPLC-MS analysis was performed at a flow rate of 0.90 mL min−1. Each alkaloid that is resolved was characterized by precursor ions and fragment ions with electrospray ionization (ESI) source in both positive and negative ionization using scan mode. The limit of detections (LODs) were 0.087, 0.727, 0.035, 0.124, 0.782 and 0.794 μg mL−1 for magnoflorine, berbamine, columbamine, jatrorrhizine, palmatine and berberine, respectively. The proposed UHPLC-PDA method was fully validated according to international (ICH) guidelines and was found to be selective, sensitive and highly accurate for the concomitant estimation of the aforementioned symbolic bio-markers of B. aristata roots.

Food ingredients hold a higher nutritional value as a botanical supplement playing a vital role in modifying and maintaining the physiological conditions that improve human health benefits. The Kashmir saffron (Crocus sativus L; KCS) obtained from dried stigmas is known for its aroma precursors and apocarotenoid derivatives, imparting a wide range of medicinal values and therapeutic benefits. In the present study, a simultaneous determination of apocarotenoids and flavonoids in stigma-based botanical supplements was carried out using analytical investigations. The high-performance thin-layer chromatography-based qualitative analysis of the raw material (stigmas, stamens, and tepals) and stigma extract has been carried out to identify apocarotenoids and flavonoids. The rapid HPLC-PDA method for the simultaneous quantification of KCS apocarotenoids was robust, precise ( 0.99), and accurate (80-110%) as per the single-laboratory validation data. Furthermore, the combined-expanded uncertainty (95%; K = 2) was calculated and found as 0.0035-0.007% (

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.

Background Ocimum genus, known as Tulsi or Basil, is a prominent botanical class in Asian culture, especially in India. The leaves have immunomodulatory, antioxidant, stress-relieving, and adaptogenic roles in traditional and modern medicine, with prominent usage in herbal teas and nutraceuticals. Objective An high-performance liquid chromatography–photodiode array (HPLC-PDA) method was developed and validated for quantification of vicenin-2, orientin, cynaroside, betulinic acid, genistein with syringic acid, rosmarinic acid, eugenol, carnosic acid, oleanolic acid, ursolic acid, luteolin, and apigenin and was confirmed using a novel electrospray ionisation-mass spectrometry (ESI-MS/MS) method in the Ocimum genus samples. Method The methodology parameters were developed on an reverse phase (RP) C18 column with a gradient elution of 1 mL/min flow rate for 0.1% o-phosphoric acid and acetonitrile at 210 and 340 nm wavelengths. Results The validation data for 13 bioactive compounds showed good linearity (r2 > 0.99) with sensitive LOD (0.034–0.684 µg/mL) and LOQ (0.100–2.068 µg/mL) with recoveries (83.66–101.53%). The results of the quantification were found to be precise (RSD, Conclusions The validated HPLC-PDA and LC-ESI-MS/MS method was found to be selective and suitable for analyzing 13 compounds in O. tenuiflorum and 12 cultivars from the Ocimum genus as a quality control tool. This method can be used in routine analysis as an inexpensive alternative to advanced techniques. Highlights This work is the first to report for vicenin-2, orientin, cynaroside, betulinic acid, and genistein, with simultaneous analysis of eight bioactive compounds in the Ocimum genus.

"Curcumin (CUR)" is the principal active phytoconstituent present in Curcuma longa (CL), also known as Turmeric, is a popular natural product used in food and dietary supplements industries. For economic advantage, CUR is manufactured synthetically. The synthetic curcumin (SC) could be mislabeled, mistaken, or mixed with natural origin CL or CL extract (CLE) or CL products for replenishing CUR. The study aimed to differentiate CLE and SC by targeting CIMP-1,i.e. (1E,4Z)-5-hydroxy-1-(3-hydroxy-4-methoxyphenyl) hexa-1,4-dien-3-one by HPLC-PDA (photodiode array) and HPTLC-DS (densitometry) based on unique patterns. The validated HPLC-PDA method for CIMP-1 and CUR in SC showed robustness and sensitivity up to 1% adulteration with recovery, precision, and linearity of compounds as per guidelines. All four compounds were identified and confirmed by ESI-MS/MS. In this research, the presence of Boron (B) found as a qualitative indicator of SC (> 250.0 mg/kg) and CLE (< 2.0 mg/kg) by ICP-MS. Further, this HPLC-PDA method was successfully applied for sixteen samples of CLE procured across India, out of which four samples showed the presence of synthetically origin curcumin. This research is the first report of simple, lab-based methods for profiling of CUR based on natural or synthetic origin and identification of SC.