Journal of Pharmaceutical Analysis

Bioautography and its scope in the field of natural product chemistry

Saikat Dewanjee, Moumita Gangopadhyay, Niloy Bhattacharya, Ritu Khanra, Tarun K. Dua

2015, (2): 75-84. doi: 10.1016/j.jpha.2014.06.002

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Medicinal plants, vegetables and fruits are the sources of huge number of bioactive lead/scaffolds with therapeutic and nutraceutical importance. Bioautography is a means of target-directed isolation of active molecules on chromatogram. Organic solvents employed in chromatographic separation process can be completely removed before biological detection because these solvents cause inactivation of enzymes and/or death of living organisms. They offer a rapid and easy identification of bioactive lead/scaffolds in complex matrices of plant extracts. Bioautography is a technique to isolate hit(s)/lead(s) by employing a suitable chromatographic process followed by a biological detection system. This review critically describes the methodologies to identify antimicrobial, antioxidant, enzyme inhibitor lead/scaffolds by employing bioautography. A significant number of examples have been incorporated to authenticate the methodologies.

Simultaneous determination of four active components in Alisma orientale (Sam.) Juz. by HPLC-DAD using a single reference standard

Yao-Wen Zhang, Qing Li, Chun-Xiao Lv, Xiu-Jia Liu, Xiao-Hui Chen, Kai-Shun Bi

2015, (2): 85-92. doi: 10.1016/j.jpha.2014.12.001

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A rapid, simple and practical high-performance liquid chromatography method coupled with diode array detector (HPLC–DAD) was developed to evaluate the quality of Alisma orientale (Sam.) Juz. through a simultaneous determination of four major active triterpenes using a single standard to determine the multi-components (SSDMCs). Alisol B 23-acetate was selected as the reference compound for calculating the relative response factors. All calibration curves showed good linearity (R240.9998) within test ranges. RSDs for intra- and inter-day of four analytes were less than 3.6% and 2.3%; the overall recovery was 92.1–110.2%(SSDMC). The proposed method was successfully applied to quantify the four components in 20 samples from different localities in China. Moreover, significant variations were demonstrated in the content of these compounds. In addition, hierarchical clustering analysis (HCA) and principal components analysis (PCA) were performed to differentiate and classify the samples based on the contents of Alisol C 23-acetate, Alisol A, Alisol A 24-acetate and Alisol B 23-acetate. This simple, rapid, low-cost and reliable HPLC–DAD method using SSDMC is suitable for routine quantitative analysis and quality control of A. orientale (Sam.) Juz.

Quantification of 17-desacetyl norgestimate in human plasma by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and its application to bioequivalence study

Ashish Saxena, Arun Kumar Gupta, V. Praveen Kumar, M. Sundaramoorthi Nainar, Manoj Bob, Ravisekhar Kasibhatta

2015, (2): 93-100. doi: 10.1016/j.jpha.2014.09.004

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A rapid and sensitive ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed and validated for the estimation of 17-desacetyl norgestimate in human plasma using solid-phase extraction technique. 17-desacetyl norgestimate D6 was used as the internal standard. Simple gradient chromatographic conditions and mass spectrometric detection enabled accurate and precise measurement of 17-desacetyl norgestimate at sub-picogram levels. The proposed method was validated for a linear range of 20–5000 pg/mL with a correlation coefficient Z 0.9988. The intra-run and inter-run precision and accuracy were within 10%. The overall recoveries for 17-desacetyl norgestimate and 17-desacetyl norgestimate D6 were 96.30%and 93.90%, respectively. The total run time was 4.5 min. The developed method was applied for the determination of the pharmacokinetic parameters of 17-desacetyl norgestimate following a single oral administration of a norgestimate and ethinyl estradiol 0.250 mg/0.035 mg tablets in 35 healthy female volunteers.

Selective and rapid determination of raltegravir in human plasma by liquid chromatography-tandem mass spectrometry in the negative ionization mode

Ajay Gupta, Swati Guttikar, Priyanka A. Shah, Gajendra Solanki, Pranav S. Shrivastav, Mallika Sanyal

2015, (2): 101-109. doi: 10.1016/j.jpha.2014.10.002

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A selective and rapid high-performance liquid chromatography–tandem mass spectrometry method was developed and validated for the quantification of raltegravir using raltegravir-d3 as an internal standard (IS). The analyte and IS were extracted with methylene chloride and n-hexane solvent mixture from 100 mL human plasma. The chromatographic separation was achieved on a Chromolith RP-18e endcapped C18 (100 mm ? 4.6 mm) column in a run time of 2.0 min. Quantitation was performed in the negative ionization mode using the transitions of m/z 443.1-316.1 for raltegravir and m/z 446.1-319.0 for IS. The linearity of the method was established in the concentration range of 2.0–6000 ng/mL. The mean extraction recovery for raltegravir and IS was 92.6% and 91.8%, respectively, and the IS-normalized matrix factors for raltegravir ranged from 0.992 to 0.999. The application of this method was demonstrated by a bioequivalence study on 18 healthy subjects.

Optimization of high pressure machine decocting process for Dachengqi Tang using HPLC fingerprints combined with the Box-Behnken experimental design

Rui-Fang Xie, Zhi-Na Shi, Zhi-Cheng Li, Pei-Pei Chen, Yi-Min Li, Xin Zhou

2015, (2): 110-119. doi: 10.1016/j.jpha.2014.07.001

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Using Dachengqi Tang (DCQT) as a model, high performance liquid chromatography (HPLC) fingerprints were applied to optimize machine extracting process with the Box–Behnken experimental design. HPLC fingerprints were carried out to investigate the chemical ingredients of DCQT; synthetic weighing method based on analytic hierarchy process (AHP) and criteria importance through intercriteria correlation (CRITIC) was performed to calculate synthetic scores of fingerprints; using the mark ingredients contents and synthetic scores as indicators, the Box–Behnken design was carried out to optimize the process parameters of machine decocting process under high pressure for DCQT. Results of optimal process showed that the herb materials were soaked for 45 min and extracted with 9 folds volume of water in the decocting machine under the temperature of 140 1C till the pressure arrived at 0.25 MPa;then hot decoction was excreted to soak Dahuang and Mangxiao for 5 min. Finally, obtained solutions were mixed, filtrated and packed. It concluded that HPLC fingerprints combined with the Box–Behnken experimental design could be used to optimize extracting process of traditional Chinese medicine (TCM).

Liquid chromatography/tandem mass spectrometry method for quantitative estimation of solutol HS15 and its applications

V. Vijaya Bhaskar, Anil Middha, Pratima Srivastava, Sriram Rajagopal

2015, (2): 120-129. doi: 10.1016/j.jpha.2014.09.002

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A rapid, sensitive and selective pseudoMRM (pMRM)-based method for the determination of solutol HS15 (SHS15) in rat plasma was developed using liquid chromatography/tandem mass spectro-metry (LC–MS/MS). The most abundant ions corresponding to SHS15 free polyethyleneglycol (PEG) oligomers at m/z 481, 525, 569, 613, 657, 701, 745, 789, 833, 877, 921 and 965 were selected for pMRM in electrospray mode of ionization. Purity of the lipophilic and hydrophilic components of SHS15 was estimated using evaporative light scattering detector (ELSD). Plasma concentrations of SHS15 were measured after oral administration at 2.50 g/kg dose and intravenous administration at 1.00 g/kg dose in male Sprague Dawley rats. SHS15 has poor oral bioavailability of 13.74% in rats. Differences in pharmacokinetics of oligomers were studied. A novel proposal was conveyed to the scientific community, where formulation excipient could be analyzed as a qualifier in the analysis of new chemical entities (NCEs) to address the spiky plasma concentration profiles.

Quantitative estimation of (-)-hinokinin, a trypanosomicidal marker in Piper cubeba, and some of its commercial formulations using HPLC-PDA

Kothapalli Haribabu, Makula Ajitha, Uppuluri Venkata Mallavadhani

2015, (2): 130-136. doi: 10.1016/j.jpha.2014.03.001

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The fruits of Piper cubeba have been used in Ayurvedic system of medicine for pain, tastelessness, painful urination and mouth diseases. Among its various chemical constituents, (-)-hinokinin, a trypanosomicidal dibenzylbutyrolactone lignan, is found in significant quantities. For quality evaluation of P. cubeba fruit and its commercial formulations, there is an urgent need to develop an analytical method based on (-)-hinokinin. For this purpose, an HPLC method was developed using photo diode array detector and Waters HR C18 column with gradient elution consisting of water and acetonitrile. The developed method was validated as per ICH-Q2B guidelines and found to be accurate, precise and linear over a wide range of concentrations (5–300 mg/mL). (-)-Hinokinin contents were found to be in the range of 0.005–0.109%(m/m) in various P. cubeba samples. The developed method was extended to LC–MS for further identification and characterization of (-)-hinokinin in samples. The developed method is simple, rapid and specific, and can be used as a tool for quality control of P. cubeba fruits and its commercial formulations.

Monolithic LC method applied to fesoterodine fumarate low dose extended-release tablets:Dissolution and release kinetics

Maximiliano S. Sangoi, Vítor Todeschini, Martin Steppe

2015, (2): 137-141. doi: 10.1016/j.jpha.2014.10.001

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A dissolution test for fesoterodine low dose extended-release tablets using liquid chromato-graphic (LC) method equipped with a C18 monolithic column was developed and validated. LC system was operated isocratically at controlled temperature (40 1C) using a mobile phase of acetonitrile:methanol:0.03 M ammonium acetate (pH 3.8) (30:15:55, v/v/v), run at a flow rate of 1.5 mL/min and detected at 208 nm. The best dissolution conditions for this formulation were achieved using a USP apparatus 2 (paddle) at 100 rpm and 900 mL of phosphate buffer at pH 6.8 as the dissolution medium. Validation parameters such as the specificity, linearity, accuracy, precision, and robustness were evaluated according to international guidelines, giving results within the acceptable range. The kinetic parameters of drug release were also investigated using model-dependent methods and the dissolution profiles were best described by the Higuchi model. The validated dissolution test can be applied for quality control of this formulation.

Application of analytical instruments in pharmaceutical analysis

2015, (2): 142-145.

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2015 Vol. 5, No. 2