Just Published: Journal of Pharmaceutical and Biomedical Analysis

A new issue of this journal has just been published. To see abstracts of the papers it contains (with links through to the full papers) click here:

Journal of Pharmaceutical and Biomedical Analysis
http://rss.sciencedirect.com/publication/science/5266

Selected papers from the latest issue:

2.

An appraisal of the chemical and thermal stability of silica based reversed-phase liquid chromatographic stationary phases employed within the pharmaceutical environment   Review Article Pages 100-115 Endler M. Borges, Melvin R. Euerby Graphical abstract Highlights ► The development of RPLC columns for the analysis of ionizable analytes is discussed. ► The thermal, chemical and mechanical stability of RPLC stationary phases are discussed. ► The development of RPLC fused core–shell technology is discussed. ► The development of RPLC sub-2μm phases is discussed. ► Effect of RPLC operating parameters on peak shape of bases.

Pharmaceutical Applications

3.

Chaotropic agents in liquid chromatographic method development for the simultaneous analysis of levodopa, carbidopa, entacapone and their impurities   Original Research Article Pages 9-15 Ana Vemić, Biljana Jančić Stojanović, Ivana Stamenković, Anđelija Malenović Graphical abstract Highlights ► LC method development for the simultaneous analysis of antiparkinsonian drugs levodopa, carbidopa, entacapone and their impurities. ► Application of chaotropic agents and effect of their anion in the manipulation of analytes retention behavior. ► Box–Behnken experimental design and Derringer's desirability function in the optimization of the gradient elution program.

4.

Simultaneous determination of 24 constituents in Cortex Lycii using high-performance liquid chromatography–triple quadrupole mass spectrometry   Original Research Article Pages 63-70 Jing-Xian Zhang, Shu-Hong Guan, Min Yang, Rui-Hong Feng, Yang Wang, Yi-Bei Zhang, Xin Chen, Xiao-Hui Chen, Kai-Shun Bi, De-An Guo Graphical abstract Highlights ► A LC–MS/MS method was established to determine 24 compounds in Cortex Lycii. ► Cyclic peptides and phenolic amides are the characteristic compounds. ► PCA was used to discriminate samples from different sources. ► The results would be helpful in the establishment of the quality standard.

5.

Measurement of acid dissociation constants and ionic mobilities of 3-nitro-tyrosine and 3-chloro-tyrosine by capillary zone electrophoresis   Original Research Article Pages 83-87 Haixia Ren, Licheng Wang, Xusheng Wang, Xia Liu, Shengxiang Jiang Graphical abstract The dissociation constant (pKa) and limiting mobility of 3-chlorotyrosine (CT) and 3-nitrotyrosine (NT) obtained were inserted into database in Peakmaster, whose prediction led to satisfactory agreement with experimental runs. Highlights ► This article reported limiting mobilities and pKavalues of 3-nitrotyrosine and 3-chlorotyrosine. ► Once tested the data in Peakmaster 5.2, satisfactory agreement with experimental results was obtained. ► The calculation was improved by a simple theoretical model instead of an empirical assumption usually used.

6.

Content determination of the major constituents of Yinchenzhufu decoction via ultra high-performance liquid chromatography coupled with electrospray ionisation tandem mass spectrometry   Original Research Article Pages 88-93 Qian Wang, Rong Shi, Yue-Ming Ma, Peng Jiang, Jie Zhong, Hong-Yan Cui, Ping Liu, Cheng-Hai Liu Graphical abstract Highlights ► Yinchenzhufu decoction has the potential to develop a new drug for treating jaundice. ► A UHPLC–MS method was established for the first time to determine the 10 compounds. ► The method was applied to quantify the compounds in different batches of samples.

7.

Determination of elemental impurities in leachate solutions from syringes using sector field ICP-mass spectrometry   Original Research Article Pages 139-144 K. Van Hoecke, C. Catry, F. Vanhaecke Graphical abstract Highlights ► Leaching of elemental impurities from glass syringes was assessed using sector field ICP-MS. ► Sixteen elements defined in draft USP chapter 232, Na, Al, Si, and W were determined. ► All leachate solutions contained Na and Si, up to 1200 and 4500μgL−1, respectively. ► Al, As and W leached in variable amounts from syringes of one manufacturer. ► Harmonization of test and limit concentration guidelines would be beneficial.

8.

Differential scanning fluorimetry: Rapid screening of formulations that promote the stability of reference preparations    Pages 163-166 Kiran Malik, Paul Matejtschuk, Craig Thelwell, Chris J. Burns Graphical abstract DSF scans of alpha-1-proteinase inhibitor with stabilising (green) and destabilising (red) excipient choices compared to control (black). Highlights ► Investigated novel and current methods for formulation of a model protein (alpha-1-proteinase inhibitor). ► Differential scanning fluorimetry (DSF) gave similar trends for the excipients chosen compared to micro DSC. ► DSF using PCR thermal cycle is convenient rapid and high throughput option for formulation selection.

9.

A metabolite-profiling approach allows the identification of new compounds from Pistacia lentiscus leaves   Original Research Article Pages 167-174 C. Rodríguez-Pérez, R. Quirantes-Piné, N. Amessis-Ouchemoukh, K. Madani, A. Segura-Carretero, A. Fernández-Gutierrez Graphical abstract A metabolite profiling of methanol extract fromPistacia Lentiscusleaves was carried out using HPLC–ESI-QTOF-MS. 46 different compounds were identified, 20 of which were tentatively characterized for the first time. Highlights ►Pistacia lentiscusleaves extract has been characterized. ► A HPLC–ESI-QTOF-MS method has been developed and validated. ► This method allowed the tentative identification of 46 compounds. ► The most representative the groups were flavonoids, phenolic acids and derivatives. ► 20 of these compounds have been tentatively identified for the first time.

Bioanalytical Applications

10.

Buprenorphine and norbuprenorphine quantification in human plasma by simple protein precipitation and ultra-high performance liquid chromatography tandem mass spectrometry   Original Research Article Pages 1-8 Guillaume Lüthi, Valeria Blangy, Chin B. Eap, Nicolas Ansermot Graphical abstract Representative chromatograms of a plasma sample of a patient taking buprenorphine. Highlights ► Buprenorphine and norbuprenorphine were quantified in plasma by UHPLC–MS/MS. ► This is the first extraction of these analytes from plasma by simple protein precipitation. ► Stable isotope-labeled IS were used to compensate for the global method variability. ► The method was highly sensitive with very good validation performances. ► This method is suitable both for pharmacokinetic studies and routine TDM.

11.

Pharmacokinetic study of major bioactive components in rats after oral administration of extract of Ilex hainanensis by high-performance liquid chromatography/electrospray ionization mass spectrometry   Original Research Article Pages 21-28 Jie Yang, Fang Lv, Xiao-qing Chen, Wei-xi Cui, Li-hong Chen, Xiao-dong Wen, Qiang Wang Graphical abstract Highlights ► A rapid, sensitive and convenient LC–MS method for simultaneous determination of chlorogenic acid, kaempferol-7-O-β-d-glucoside, and ilexgenin A in plasma was developed and validated. ► The method was applied to pharmacokinetics after oral administration of extract ofIlex hainanensisto rats. ► The differences of their pharmacokinetic behaviors in normal and NAFLD rats were investigated.

12.

Alkyl chain dependent interactions of ligands with bovine serum albumin   Original Research Article Pages 55-62 Nihar Dash, Anasuya Mishra, G. Krishnamoorthy Graphical abstract Highlights ► A kinase inhibitor and its alkylated products interactions with BSA are studied. ► Weakly fluorescent molecules become strongly fluorescent upon binding with BSA. ► Kinase inhibitor and its pyridine nitrogen alkylated product bind at hydrophobic site. ► Imidazole nitrogen alkylated product binds at the hydrophilic site. ► Imidazole nitrogen alkylated product induces conformational change in BSA.

13.

Development of a UFLC–MS/MS method for simultaneous determination of six lignans of Schisandra chinensis (Turcz.) Baill. in rat plasma and its application to a comparative pharmacokinetic study in normal and insomnic rats   Original Research Article Pages 120-127 Binbin Wei, Qing Li, Dan Su, Ronghua Fan, Longshan Zhao, Lulu Geng, Bosai He, Xiaohui Chen, Ying Jia, Kaishun Bi Graphical abstract Schisandrin (I), schisandrol B (II), schisantherin A (III), deoxyshisandrin (IV),γ-schisandrin (V-1), gomisin N (V-2) and bifendate (VI; IS). Highlights ► Simultaneous determination of six lignans in rat plasma. ► The total analysis time was 11.0min ► LLOQ were 10, 1.2, 1.2, 1.2, 1.0 and 1.2ngmL−1for the analytes. ► We compared pharmacokinetic profiles of analytes in normal and insomnic rats.

14.

Determination of diosbulbin B in rat plasma and urine by LC–MS/MS and its application in pharmacokinetic and urinary excretion studies   Original Research Article Pages 133-138 Yujuan Li, Yuan Tian, Lin Gan, Yongzhi Li, Bo Chen, Jinyuan Qiao Graphical abstract Product ion mass spectra of [M+Na]+ion of (A) diosbulbin B and [M+H]+ion of (B) buspirone (IS). Highlights ► LC–MS method was developed for determination of diosbulbin B in rat plasma and urine. ► Pharmacokinetic parameters of diosbulbin B were firstly reported in rats. ► Urinary excretion results of diosbulbin B in rat were reported for the first time.

15.

Rapid analysis of tadalafil in human blood plasma and seminal plasma by liquid chromatography/tandem mass spectrometry   Original Research Article Pages 149-157 Bo Ma, Xuejun Shang, Qi Zhang, Jing Li, Yinhui Liu, Xiaomei Cao, Qiuyu Xu Graphical abstract Highlights ► Rapid analysis of tadalafil in human plasma and seminal plasma by LC–MS/MS. ► This method was applied in a single dose pharmacokinetic study. ► Tadalafil levels in seminal plasma were firstly reported in Chinese human. ► The correlation study of tadalafil levels in human plasma and seminal plasma.

Short Communications

16.

Multivariate detection limits of on-line NIR model for extraction process of chlorogenic acid from Lonicera japonica    Pages 16-20 Zhisheng Wu, Chenglin Sui, Bing Xu, Lu Ai, Qun Ma, Xinyuan Shi, Yanjiang Qiao Graphical abstract A methodology is proposed to estimate the multivariate detection limits (MDL) of on-line near-infrared (NIR) model for extraction process of chlorogenic acid fromLonicera japonica. Highlights ► Multivariate detection limits of on-line NIR model were given. ► On-line monitoring of extraction process was investigated usingLonicera japonica. ► NIR band of chlorogenic acid compound was assigned by deuterated solution.

17.

Simultaneous determination of phosphate anion and calcium cation in Plastrum testudinis by HPLC–ELSD    Pages 29-31 Qingfa Tang, Xinyu Wang, Feilong Chen, Xiaomei Tan Graphical abstract HPLC–ELSD simultaneous analysis of phosphate anion and calcium cation inPlastrum testudinis. Highlights ► HPLC–ELSD method was validated for the quantification of phosphate anion and calcium cation inPlastrum testudinis. ► Provide a method was successfully applied for quality assessment of inorganic compound in TCM. ► The method is simple, fast, and sensitive.

18.

Macrophage biospecific extraction and HPLC–ESI-MSn analysis for screening immunological active components in Smilacis Glabrae Rhizoma    Pages 44-48 Zhao-Guang Zheng, Ting-Ting Duan, Bao He, Dan Tang, Xiao-Bin Jia, Ru-Shang Wang, Jia-Xiao Zhu, You-Hua Xu, Quan Zhu, Liang Feng Graphical abstract Highlights ► To screen immunological active components fromSmilacis Glabrae Rhizoma. ► Transwell inserts offer advantages for extracting biospecific active components from TCM by cells. ► Compounds extracted by macrophages have been proved to possess immunological activity.

19.

RP-HPLC separation and ESI-MS, 1H, and 13C NMR characterization of forced degradants including process related impurities of carisbamate: Method development and validation    Pages 49-54 Ramisetti Nageswara Rao, Kuntamukkala Ramakrishna, Bompelli Sravan, Kondapalli Santhakumar Graphical abstract Chemical structure and molecular formula of carisbamate. Highlights ► First RP-HPLC stability indicating method for carisbamate, an anti-epileptic drug. ► First explanation to isomerization of carisbamate under acid and base hydrolysis. ► First report on McLafferty type of rearrangement in carisbamate and its isomer. ► Synthesis, isolation and characterization of carisbamate and its related substances.

20.

Simultaneous determination of scopoletin, psoralen, bergapten, xanthotoxin, columbianetin acetate, imperatorin, osthole and isoimperatorin in rat plasma by LC–MS/MS for pharmacokinetic studies following oral administration of Radix Angelicae Pubescentis extract    Pages 71-75 Yan-xu Chang, Qiu-Hong Zhang, Jin Li, Ling Zhang, Xin-rong Guo, Jun He, Peng Zhang, Lin Ma, Yan-ru Deng, Bo-li Zhang, Xiu-mei Gao Graphical abstract Mean plasma concentration versus time profiles in rats after oral administration of 6gkg−1CAngelicae Pubescentis Radix. Highlights ► An LC–MS/MS method was developed and validated for determination of coumarins. ► The lower limits of quantitations of eight coumarins were lower than 2.16ngmL−1. ► It was sensitive to study pharmacokinetic of Radix Angelicae Pubescentis extract. ► The main pharmacokinetic parameters of coumarins of RAP in rats were reported.

21.

Development of an analytical method for the quantification of pfaffic acid in Brazilian ginseng (Hebanthe eriantha)    Pages 76-82 Marili Villa Nova Rodrigues, Kelly de Paula Souza, Vera Lucia Garcia Rehder, Gisele Freitas Vilela, Ílio Montanari Júnior, Glyn Mara Figueira, Susanne Rath Graphical abstract Highlights ► A HPLC-DAD method for the determination of pfaffic acid was developed and validated. ► Pfaffic acid is an active marker ofHebanthe eriantha. ► Hydrolysis conditions were optimized using a central composite experimental design. ► The proposed method is a useful tool in the quality control of Brazilian ginseng.

22.

Evaluating MISER chromatography for a rapid formulation screen    Pages 94-99 Robert Papp, Ulrika Andersson, Louis-David Cantin Graphical abstract Highlights ► A rapid miniaturized formulation screen was developed to identify dosing vehicles. ► MISER chromatography was evaluated to increase processing speed. ► The benefits and challenges of implementing MISER are discussed. ► MISER provides a suitable reporting format eliminating many data processing steps.

23.

Investigation of thermal decomposition of ascorbic acid by TG-FTIR and thermal kinetics analysis    Pages 116-119 Shi Jingyan, Liu Yuwen, Wang Zhiyong, Wang Cunxin Graphical abstract Highlights ► TG-FTIR was used to investigate the thermal behavior of ascorbic acid. ► Dry solid ascorbic acid begin to decompose at 191°C and the decomposition process consists of three stages in the temperature range of 191–800°C. ► Five species of evolved gases CO2, CO, H2O, CH4and HCOOH were detected, in which HCOOH was identified for the first time. ► The isoconversional method and the master plots method were applied to thermal kinetic analysis. ► The first stage of ascorbic acid decomposition can be described by the model of 1st order reaction.

24.

Effects of borneol on the pharmacokinetics of geniposide in cortex, hippocampus, hypothalamus and striatum of conscious rat by simultaneous brain microdialysis coupled with UPLC–MS    Pages 128-132 Bin Yu, Ming Ruan, Xiao-bing Cui, Jian-Ming Guo, Li Xu, Xiao-Ping Dong Graphical abstract Highlights ► We monitored the concentration of geniposide from four brain regions of conscious rat. ► A microdialysis combining with an efficient UPLC–MS method was adopted. ► The delivery of geniposide in cortex was more than that in other regions in physiological status. ► Borneol increased the delivery of geniposide in hippocampus and hypothalamus. ► Borneol affect the opening of BBB in a region specific manner.

25.

The case of Hypericum rochelii Griseb. & Schenk and Hypericum umbellatum A. Kern. essential oils: Chemical composition and antimicrobial activity    Pages 145-148 Aleksandra Đorđević, Jelena Lazarević, Andrija Šmelcerović, Gordana Stojanović Graphical abstract Highlights ► Composition of the volatiles isolated from twoHypericumtaxa was evaluated. ► One hundred and forty-three constituents were identified in both oils. ► The antimicrobial activity was examined by microdilution method. ► We report chemical composition and antimicrobial activity for the first time.

26.

Determination of nicousamide in human plasma by liquid chromatography–tandem mass spectrometry    Pages 158-162 Wenyuan Qi, Qian Zhao, Hongzhong Liu, Ji Jiang, Xiaoguang Chen, Pei Hu Graphical abstract Highlights ► A sensitive LC–MS/MS method for quantify nicousamide in human plasma was developed and fully validated. ► Only 100μL plasma was required for the sample pretreatment procedures. ► The overall run time was 1.5min, that allow to analyze large sample in a short time. ► The method had been successfully applied in the clinical study of nicousamide.

Miscellaneous

27.

Near infrared spectroscopy in combination with chemometrics as a process analytical technology (PAT) tool for on-line quantitative monitoring of alcohol precipitation   Original Research Article Pages 32-39 Ye Jin, Zengzeng Wu, Xuesong Liu, Yongjiang Wu Graphical abstract Highlights ► NIR spectroscopy was applied to on-line monitoring of alcohol precipitation. ► PSO was used to optimize the hyper-parameters of LS-SVM model. ► LS-SVM and PLS models were developed for five critical quality attributes. ► PSO based LS-SVM provided slightly better fitting results and prediction accuracy.

28.

The uncertainty of purity of reference materials must be known   Original Research Article Pages 40-43 Rodrigo Borges, Veronika R. Meyer Highlights ► Measurement uncertainty is an essential part of analytical results. ► Measurement uncertainty can only be calculated if the content uncertainty of the reference materials is known. ► A reference material needs not necessarily to be of highest purity, but the uncertainty of its content must be known. ► The situation with reference materials of pharmaceutical interest is unsatisfactory.

29.

Identification of cytochrome P450 isoenzymes involved in metabolism of (+)-praeruptorin A, a calcium channel blocker, by human liver microsomes using ultra high-performance liquid chromatography coupled with tandem mass spectrometry   Original Research Article Pages 175-188 Wang-Hui Jing, Yue-Lin Song, Ru Yan, Yi-Tao Wang Graphical abstract Highlights ►dPA metabolic kinetics in HLMs was determined by UHPLC–MS/MS for the first time. ► Contribution of CYPs was evaluated using inhibitors and recombinant human CYPs. ► CYP3A4 is proved to be the main isoform mediating both hydrolysis and oxidation. ► Oxidation at C-3′ side chain ofdPA was consolidated with NMR spectrometry.