scholarly journals Validated Chromatographic methods for estimation of Solanine in Mahamrutyunjaya rasa

2020 ◽  
Vol 2 (01) ◽  
Author(s):  
Pallavi Rai ◽  
Rahul Kaushik ◽  
Sadhana J. Rajput
Keyword(s):  
High Performance ◽  
Reversed Phase ◽  
Therapeutic Window ◽  
Chromatographic Methods ◽  
Linearity Range ◽  
Ich Guidelines ◽  
Ld50 Value ◽  
Layer Chromatography ◽  
Chloroform Methanol ◽  
Solanum Indicum

Introduction: Mahamrutyunjaya rasa is a herbomineral ayurvedic formulation used for various indications like fever, pain, cardiac arrhythmia, etc. It contains Solanum indicum as one of the ingredients having anti-inflammatory, diuretic, and diaphoretic properties. Solanine is one of the active biomarkers for Solanum indicum. The therapeutic window of Solanine is very narrow, with the LD50 value of 3-6 mg/kg body weight in humans. Objective: Estimation of such biomarkers is very significant to avoid any adverse events due to the administration of ayurvedic preparations containing Solanine. In the present study, two simple, sensitive, reliable chromatographic techniques have been developed and validated for the estimation of Solanine in Mahamrutyunjaya rasa. Materials and Methods: High-performance liquid chromatography (HPLC) separation of Solanine was performed on an reversed phase C-18 column (250 mm 9 4.6 mm ID, 5 lm particle size), with isocratic elution using a mixture of Tris buffer (10mM, pH 6.00): Acetonitrile(60:40, v/v) at a flow rate of 1 mL/min with UV detection at 218 nm for solanine. High-performance thin-layer chromatography (HPTLC) separation was done on Silica gel 60 F254 pre-coated plates using Chloroform: Methanol: Ammonia (7:3:0.5 v/v). The densitometric scanning was performed at 500 nm. The developed methods were validated for linearity, LOD, LOQ, accuracy, precision, and specificity as per ICH guidelines. Results: Solanine was eluted at 4.43 ± 0.1 min and established a linearity range of 1 – 100 μg/ml (r2 = 0.9992). In the HPTLC method, the Rf value of Solanine was 0.05 in a linearity range of 1600-4800 ng/ml. Conclusion: Reliable, rapid, simple, and sensitive chromatographic methods were developed for the quantification of Solanine in Mahamrutyunjaya Rasa.

Two Validated Chromatographic Methods for Determination of Ciprofloxacin HCl, One of its Specified Impurities and Fluocinolone Acetonide in Newly Approved Otic Solution

2021 ◽  
Author(s):  
Mahmoud A Tantawy ◽  
Israa A Wahba ◽  
Samah S Saad ◽  
Nesrin K Ramadan
Keyword(s):  
High Performance ◽  
Fluocinolone Acetonide ◽  
Ultraviolet Detection ◽  
Chromatographic Methods ◽  
Bulk Powder ◽  
Developing System ◽  
Layer Chromatography ◽  
Chloroform Methanol ◽  
Linear Regressions

Abstract Two sensitive, selective and precise chromatographic methods have been established for concomitant quantification of ciprofloxacin HCl (CIP), fluocinolone acetonide (FLU) along with ciprofloxacin impurity A (CIP-imp A). The first method was thin-layer chromatography (TLC-densitometry) where separation was accomplished using TLC silica plates 60 G.F254 as a stationary phase and chloroform–methanol–33%ammonia (4.6:4.4:1, by volume) as a developing system. The obtained plates were scanned at 260 nm over concentration ranges of 1.0–40.0, 0.6–20.0 and 1.0–40.0 μg band−1 for CIP, FLU and CIP-imp A, respectively. The second method was based on high-performance liquid chromatography using a Zorbax ODS column (5 μm, 150 × 4.6 mm i.d.) where adequate separation was achieved through a mobile phase composed of phosphate buffer pH 3.6–acetonitrile (45:55, v/v) at flow rate 1.0 mL min−1 with ultraviolet detection at 254 nm. Linear regressions were obtained in the range of 1.0–40.0 μg mL−1 for CIP, 0.6–20.0 μg mL−1 for FLU and 1.0–40.0 μg mL−1 for CIP-imp A. The suggested methods were validated in compliance with the International Conference on Harmonization guidelines and were successfully applied for determination of CIP and FLU in bulk powder and newly marketed otic solution.

scholarly journals Rapid, Highly-Sensitive and Ecologically Greener Reversed-Phase/Normal-Phase HPTLC Technique with Univariate Calibration for the Determination of Trans-Resveratrol

Separations ◽  
2021 ◽  
Vol 8 (10) ◽  
pp. 184
Author(s):  
Prawez Alam ◽  
Faiyaz Shakeel ◽  
Mohammed H. Alqarni ◽  
Ahmed I. Foudah ◽  
Mohammed M. Ghoneim ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Normal Phase ◽  
Commercial Formulation ◽  
Highly Sensitive ◽  
Validation Parameters ◽  
Layer Chromatography ◽  
Chloroform Methanol

The rapid, highly-sensitive and ecologically greener reversed-phase (RP)/normal-phase (NP) high-performance thin-layer chromatography (HPTLC) densitometric technique has been developed and validated for the determination of trans-resveratrol (TRV). The reversed-phase HPTLC-based analysis of TRV was performed using ethanol–water (65:35, v v−1) combination as the greener mobile phase, while, the normal-phase HPTLC-based estimation of TRV was performed using chloroform–methanol (85:15, v v−1) combination as the routine mobile phase. The TRV detection was carried out at 302 nm for RP/NP densitometric assay. The linearity was recorded as 10–1200 and 30–400 ng band−1 for RP and NP HPTLC techniques, respectively. The RP densitometric assay was observed as highly-sensitive, accurate, precise and robust for TRV detection in comparison with the NP densitometric assay. The contents of TRV in commercial formulation were recorded as 101.21% utilizing the RP densitometric assay, while, the contents of TRV in commercial formulation were found to be 91.64% utilizing the NP densitometric assay. The greener profile of RP/NP technique was obtained using the analytical GREEnness (AGREE) approach. The AGREE scales for RP and NP densitometric assays were estimated 0.75 and 0.48, respectively. The recorded AGREE scale for the RP densitometric assay indicated that this technique was highly green/the ecologically greener compared to the NP densitometric assay. After successful optimization of analytical conditions, validation parameters, AGREE scale and chromatography performance, the RP densitometric assay with univariate calibration was found to be better than the NP densitometric assay for the analysis of TRV.

scholarly journals Fingerprint Study of Curcuma xanthorrhiza Rhizome by High Performance Thin Layer Chromatography (HPTLC)

2016 ◽  
Vol 1 (2) ◽  
pp. 9-14
Author(s):  
Tina Wikara ◽  
Anny Sulistiowaty ◽  
Sri Murhandini ◽  
Tepy Usia
Keyword(s):  
High Performance ◽  
Phytochemical Analysis ◽  
Hptlc Plate ◽  
Spot Detection ◽  
Ich Guidelines ◽  
Curcuma Xanthorrhiza ◽  
Layer Chromatography ◽  
Chloroform Methanol

The rhizome of Curcuma xanthorrhiza Roxb is intensively used in Indonesia as traditional medicine. It is widely used for hepatoprotective and anti inflammatory activities. To ensure the quality of its extract, we have studied the fingerprint or phytochemical analysis. This research was aimed to produce a chromatogram profile of the rhizome by HPTLC. The HPTLC fingerprint chromatogram of C. xanthorrhiza rhizome was performed using HPTLC plate of silica gel 60 F254 as the stationary phase and chloroform-methanol (97:3) as the mobile phase. Spot detection was carried out by TLC photo documentary system at 254 and 366 nm and TLC scanner at 427 nm. The developed method was validated according to ICH guidelines by determination of specificity and precision. We found that the specifity and precission of the method were met the acceptance criteria. In conclusion, the developed method is valid and could be used for quality control and standardization of herbal medicine containing C. xanthorrhiza rhizome.

Development and Validation of Chromatographic Methods for Simultaneous Determination of Paracetamol, Orphenadrine Citrate and Caffeine in Presence of P-aminophenol; Quantification of P-aminophenol Nephrotoxic Impurity Using LC–MS/MS

2019 ◽  
Vol 58 (3) ◽  
pp. 223-233 ◽  
Author(s):  
Shereen A Boltia ◽  
Aya T Soudi ◽  
Eman S Elzanfaly ◽  
Hala E Zaazaa
Keyword(s):  
High Performance ◽  
Reversed Phase ◽  
Limit Of Quantification ◽  
Chromatographic Methods ◽  
Ich Guidelines ◽  
Positive Mode ◽  
Tlc Plates ◽  
Array Detection ◽  
Development And Validation ◽  
Developing System

Abstract Three chromatographic methods were developed, optimized and validated for Paracetamol (PAR), Orphenadrine citrate (Or.cit) and Caffeine (CAF) determination in their mixture and in presence of PAR toxic impurity; P-aminophenol (PAP) in tablets. The first method is based on a thin layer chromatography combined with densitometry. Separation was achieved using silica gel 60 F254 TLC plates and dichloromethane:methanol:acetone:glacial acetic acid (9:1:0.5:0.3, v/v/v) as a developing system at 230 nm. The second method is based on high-performance liquid chromatography with diode array detection. The proposed compounds are separated on a reversed phase C18 analytical column using phosphate buffer (pH 9; 0.05 M) and methanol (80:20, v/v) at 1.2 mL/min. Linear regressions are obtained in the range of 1–500 μg/mL, 25–1000 μg/mL and 1–400 μg/mL for PAR, Or.cit and CAF, respectively. Quantification of the toxic PAP is carried out using LC–MS-MS by electrospray ionization in the positive mode using triple quadrupole mass spectrometry. The limit of quantification for PAP is 1 ng/mL. All methods are validated according to the ICH guidelines and successfully applied to determine PAR, Or.cit, CAF and PAP in pure powder and in combined tablets dosage form without interference from excipients.

scholarly journals Chromatographic methods for determination of finasteride and tamsulosin hydrochloride and in presence of finasteride degradation product

2020 ◽  
Vol 32 (2) ◽  
pp. 95-101 ◽  
Author(s):  
Hany H. Monir ◽  
Alshimaa M. Ali ◽  
Rawnaa E. Refat ◽  
Samah S. Abbas
Keyword(s):  
Degradation Product ◽  
High Performance ◽  
Uv Detection ◽  
Hplc Separation ◽  
Chromatographic Methods ◽  
Bulk Powder ◽  
Ich Guidelines ◽  
Aluminum Plates ◽  
Layer Chromatography

Two sensitive and selective chromatographic methods were developed for determination of finasteride and tamsulosin hydrochloride in bulk powder and a pharmaceutical formulation. The first method was based on high-performance liquid chromatography (HPLC) separation of the cited drugs in the presence of the acid degradation product of finasteride. The separation was achieved using a C18 column (300 mm × 3.9 mm; 10-μm particle size) and a mobile phase consisting of 0.04 M ortho-phosphoric acid (pH 3.5 ± 0.2 adjusted with triethylamine) and acetonitrile (50:50, v/v). Quantification was achieved with ultraviolet (UV) detection at 215 nm. Linearity was in the range of 10.00–110.00 μg/mL and 2.00–44.00 μg/mL for finasteride and tamsulosin hydrochloride, respectively. Thin-layer chromatography (TLC)–densitometric method was achieved on an aluminum plates pre-coated with silica gel 60 F254 using toluene–ethanol–diethylamine (8:2:1.5, by volume) as eluent, and the RF values of tamsulosin hydrochloride and finasteride were 0.57 and 0.64, respectively. Quantification was achieved with UV detection at 250 nm for finasteride and 280 nm for tamsulosin hydrochloride. Linearity was in the range of 1.00–40.00 and 0.2.00–20.00 μg per spot for finasteride and tamsulosin hydrochloride, respectively. The results obtained were validated according to the International Conference on Harmonisation (ICH) guidelines. A statistical comparison between the obtained results and the results of a reported method was carried out.

scholarly journals Fingerprint Study of Curcuma xanthorrhiza Rhizome by High Performance Thin Layer Chromatography (HPTLC)

2016 ◽  
Vol 1 (2) ◽  
pp. 9-14 ◽  
Author(s):  
Tina Wikara ◽  
Anny Sulistiowaty ◽  
Sri Murhandini ◽  
Tepy Usia
Keyword(s):  
High Performance ◽  
Phytochemical Analysis ◽  
Hptlc Plate ◽  
Spot Detection ◽  
Ich Guidelines ◽  
Curcuma Xanthorrhiza ◽  
Layer Chromatography ◽  
Chloroform Methanol

The rhizome of Curcuma xanthorrhiza Roxb is intensively used in Indonesia as traditional medicine. It is widely used for hepatoprotective and anti inflammatory activities. To ensure the quality of its extract, we have studied the fingerprint or phytochemical analysis. This research was aimed to produce a chromatogram profile of the rhizome by HPTLC. The HPTLC fingerprint chromatogram of C. xanthorrhiza rhizome was performed using HPTLC plate of silica gel 60 F254 as the stationary phase and chloroform-methanol (97:3) as the mobile phase. Spot detection was carried out by TLC photo documentary system at 254 and 366 nm and TLC scanner at 427 nm. The developed method was validated according to ICH guidelines by determination of specificity and precision. We found that the specifity and precission of the method were met the acceptance criteria. In conclusion, the developed method is valid and could be used for quality control and standardization of herbal medicine containing C. xanthorrhiza rhizome.

An efficient biotransformation of progesterone into 11α-hydroxyprogesterone by Rhizopus microsporus var. oligosporus

2018 ◽  
Vol 74 (1-2) ◽  
pp. 9-15
Author(s):  
Bahman Nickavar ◽  
Hossein Vahidi ◽  
Mehrnoosh Eslami
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Time Course ◽  
Main Product ◽  
Fermented Foods ◽  
Rhizopus Microsporus ◽  
Chromatographic Methods ◽  
Anti Inflammatory ◽  
Layer Chromatography

Abstract Rhizopus microsporus var. oligosporus is a fungus that belongs to the Mucoraceae family that is used for the preparation of some soy-fermented foods. Microbial biotransformation of progesterone by R. microsporus var. oligosporus afforded some monohydroxylated and dihydroxylated metabolites. The main product was purified using chromatographic methods and identified as 11α-hydroxyprogesterone on the basis of its spectroscopic features. Time course studies by high-performance thin-layer chromatography demonstrated that this fungi efficiently hydroxylated progesterone at the 11α-position for 3 days with a yield of 76.48%, but beyond this time, the microorganism transformed 11α-hydroxyprogesterone into dihydroxylated metabolites. 11α-Hydroxyprogesterone is widely used as a precursor in the synthesis of hydrocortisone and other steroidal anti-inflammatory agents.

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