# Chromatographia (CHROMATOGRAPHIA)

Publisher: Springer Verlag

## Journal description

The ever increasing demands on the analyst make the rapid communication of new techniques and developments in the field of analytical chemistry of prime importance. CHROMATOGRAPHIA has been fulfilling this function for chromatography since it was first founded in 1968. During the intervening years, however, the journal has itself evolved to meet the challenges of changing times and demands. Thus, the composition of the Editorial Board is reviewed at regular intervals so as to reflect shifts in interest and the establishment of centres of excellence in countries that have not previously been active in the field. Publishing policy, including the number of papers and the format, are subject to continuous appraisal.

## Impact Factor Rankings

2016 Impact Factor Available summer 2017 1.411 1.37 1.437 1.195 1.075 1.098 1.312 1.145 1.171 0.959 1.145 1.145 1.23 1.317 1.619 1.741 1.844 2.079 1.869 1.438 1.885 1.601 1.573

## Impact factor over time

Impact factor
.
Year

5-year impact 1.19 8.10 0.20 0.01 0.26 Chromatographia website Chromatographia (Online) 0009-5893 38523635 Document, Periodical, Internet resource Internet Resource, Computer File, Journal / Magazine / Newspaper

## Publisher details

• Pre-print
• Author can archive a pre-print version
• Post-print
• Author can archive a post-print version
• Conditions
• Author's pre-print on pre-print servers such as arXiv.org
• Author's post-print on author's personal website immediately
• Author's post-print on any open access repository after 12 months after publication
• Publisher's version/PDF cannot be used
• Published source must be acknowledged
• Must link to publisher version
• Set phrase to accompany link to published version (see policy)
• Articles in some journals can be made Open Access on payment of additional charge
• Classification
green

## Publications in this journal

• ##### Article: Fast determination of 1-methyl-1H-1,2,4-triazole in soils contaminated by rocket fuel using solvent extraction, isotope dilution and GC-MS
Bulat Kenessov · Zhailaubay Zhubatov · Nadezhda V. Bakaikina · Alma O. Bimaganbetova · Nurlan Akynbayev · Inal Bakhytkyzy

No preview · Article · Feb 2016 · Chromatographia
• ##### Article: Extraction and Derivatization of Chlorophenoxy Acid Pesticides: Performing Two DLLME with One Extracting Phase
[Hide abstract]
ABSTRACT: A novel, simple and convenient method based on dispersive liquid–liquid microextraction (DLLME) and derivatization was developed and applied for isolation of a couple of selected chlorophenoxy acid herbicides from aquatic media. In the first step, analytes were extracted from acidic media into carbon tetrachloride phase using a DLLME. In following, derivatization was carried out on extracted compounds by means of methylation with an acidic methanol solution to increase their volatility and detectability in gas chromatography analysis. Finally, the derivatized analytes were re-extracted in the carbon tetrachloride phase in the second DLLME. Some important extraction parameters such as the nature and volume of the extraction solvent, disperser solvent, pH and the ionic strength were optimized. Subsequently, the developed method was validated by gas chromatography–mass spectrometry (GC–MS). Under the optimum conditions, the linearity was studied at the concentration range of 1–100 µg L−1 with a satisfactory coefficient of determination (r 2 > 0.99) for all the studied analytes. Also, the relative standard deviations (RSD %) values were from 2.5 to 4.5 % at the concentration levels of 2 and 50 µg L−1. The detection limits were found to be in the range of 0.15–0.31 µg L−1 using time-scheduled selected ion monitoring (SIM) mode. The developed method was successfully applied to the extraction and determination of chlorophenoxy acid herbicides in the river and tap water samples.
No preview · Article · Feb 2016 · Chromatographia
• ##### Article: Dried Blood Spots on Carboxymethyl Cellulose Sheets: Rapid Sample Preparation Based on Dissolution and Precipitation
[Hide abstract]
ABSTRACT: This short communication describes the use of carboxymethyl cellulose sheets as sampling material for dried blood spots. Whole blood, spiked with quetiapine, a hydrophobic and basic small molecule drug substance, was spotted on the sheet and subsequently dried. The dried spot was then almost completely dissolved in acidified aqueous solution. It was shown that the dissolved polymer, together with major blood components can easily be precipitated and removed with acetonitrile. The presented sampling on a water-soluble biopolymer derivative followed by precipitation resulted in a simple protocol and around 100 % recovery of the analyte prior to liquid chromatography—tandem mass spectrometry.
No preview · Article · Feb 2016 · Chromatographia
• ##### Article: Comparison of the Hydrolysis and Esterification Methods for the Determination of Genotoxic 5-Chlorothiophene-2-Carbonyl Chloride in Rivaroxaban Using HPLC
[Hide abstract]
ABSTRACT: This paper describes the development and comparison of the hydrolysis and esterification methods for the determination of 5-chlorothiophene-2-carbonylchloride (CTCC), a potential genotoxic impurity, in the drug rivaroxaban (RIVA) drug substance. Poor recovery of CTCC in the hydrolysis method occurred due to the high percentage of acetonitrile, which suppressed the hydrolysis reaction, but was solved by adding Na2CO3. In the esterification approach, the problem of poor recovery was also encountered because of the competition between the hydrolysis and esterification reactions, and a stable recovery of CTCC under different water content conditions was obtained by adding glacial acetic acid. A high-performance liquid chromatography (HPLC) method was developed to separate the hydrolysis product, 5-chlorothiophene-2-carboxylic acid (CTCA), and the esterification product, methyl-5-chlorothiophene-2-carboxylate (MCTC), from RIVA, process-related impurities and degradation products of RIVA. Standard curves were linear (r = 0.9999) for the hydrolysis and esterification methods in the ranges of 16.7–280.3 ppm and 15.3–255.0 ppm, respectively, and limit of quantitation (LOQ) of CTCA and MCTC was 16.7 and 15.3 ppm, respectively. The accuracy (% recovery) was 98.08–100.5 % for the hydrolysis method and 97.86–99.05 % for the esterification method. Both methods had good repeatability and stability. During the real sample analysis, it was found that the hydrolysis method could not differentiate CTCC and the inherent CTCA impurity, leading to overestimation of residual CTCC in the RIVA. The esterification method was a better solution for the accurate measurement of residual CTCC in RIVA.
No preview · Article · Feb 2016 · Chromatographia
• ##### Article: Colin P. Summerhayes: Earth’s Climate Evolution

No preview · Article · Feb 2016 · Chromatographia
• ##### Article: Metabolite Profiling to Monitor Organochlorine Pesticide Exposure in HepG2 Cell Culture
[Hide abstract]
ABSTRACT: Gas chromatography coupled with time of flight mass spectrometry (GC/MS-TOF) was used to profile endogenous metabolites in HepG2 cell cultures to assess the metabolic changes induced by exposure to different organochlorine pesticides, their mixtures and controls (endosulfan, lindane, DDT and aldrin). Cells were cultured in DMEM with Glutamax at 37 °C with 5 % CO2 for 72 h and then exposed to each pesticide, pesticide mixture or DMSO (as a control) for 24 h, and finally, endogenous metabolites were extracted and analyzed using GC/MS-TOF. The experiment was repeated six times under the same cell passage and culture conditions. PCA, PLS-DA and ROC were performed to analyze the GC/MS-TOF data and identify potential biomarkers. Thirty-five explanatory metabolites were found in both PCA and PLS-DA models, where Q 2 was 0.86 and R 2 was 0.98. Univariate and multivariate ROC showed potential biomarkers for each treatment, suggesting a general toxic mechanism for organochlorine pesticides that is specific for each type of compound. These results confirmed the effect of OCPs in sugar and amino acid metabolism that are linked with the function of cytochrome P450 in reductive dechlorination and oxidative stress.
No preview · Article · Feb 2016 · Chromatographia
• ##### Article: Simultaneous Sensitive Determination of Eight Collagen-Related Bone Turnover Biomarkers in Diverse Clinical Samples by HPLC with Fluorescent Derivatization
[Hide abstract]
ABSTRACT: The suitability of HPLC with fluorescent derivatization for simultaneous determination of eight collagen-related bone turnover biomarkers, 4-hydroxy-l-proline (OHP), pyridinoline (PYD), hydroxylysine (Hyl), deoxypyridinoline, and their glycosides, galactosyl-Pyd (Gal-Pyd, GP), galactosyl-glucosyl-Pyd, β-1-galactosyl-O-hydroxylysine (Gal-Hyl, GH), and α-1,2-glucosyl-galactosyl-O-hydroxylysine (GGH), in diverse clinical samples was investigated. 5-Carboxyfluorescein succinimidyl ester (CFSE) was chosen as the fluorescent labeling reagent. Various parameters affecting derivatization and separation were optimized. Under optimal conditions, maximum derivatization could be achieved in 25 min at 30 °C, and complete baseline separation could be completed within 25 min, with relative standard deviation values for corrected peak areas less than 3.5 % for intraday assay and 4.2 % for interday assay, respectively. The limits of detection were determined to be 0.1–1.7 nM, which are well below the expected concentrations in the real samples. The method has been used for the quantitative determination of eight target analytes in various clinical samples, including cell cultures of normal human osteoclast, preosteoblast, osteoclastoma cells and serum and urine fluids from patients with fracture, osteitis fibrosa, or osteoclastoma as well as healthy subjects, with spiked recoveries of 96–103 %. This original application of HPLC–fluorescence detection represents a powerful tool for investigating the dynamics of metabolic imbalance of these biomarkers for bone turnover under physiological and pathophysiological conditions.
No preview · Article · Feb 2016 · Chromatographia
• ##### Article: Field-Amplified Sample Injection-Capillary Electrophoresis for the Determination of Bisphenol A, α-Naphthol and β-Naphthol in Drinks and Lake Water
[Hide abstract]
ABSTRACT: To improve the sensitivity of capillary electrophoresis, field-amplified sample injection (FASI) was developed to determine bisphenol A (BPA), α-naphthol (α-NAP) and β-naphthol (β-NAP) in drinks and lake water. Parameters (sample matrix, concentration of NaCl, water plug length, sample injection time and voltage) affecting FASI have been systematically investigated. Under optimum conditions, the sensitivity was improved 17.1-, 15.8- and 9.9-fold for BPA, α-NAP and β-NAP, respectively. The detection limits of BPA, α-NAP and β-NAP were 0.071, 0.038 and 0.081 μg mL−1 and the proposed method has been successfully applied to detect BPA, α-NAP and β-NAP in drinks and lake water with recoveries of 82.0–109.3 %.
No preview · Article · Feb 2016 · Chromatographia
• ##### Article: Isolation of (Five) Steviol Glycosides from a Stevia rebaudiana Formulation by Gradient Elution Countercurrent Chromatography
[Hide abstract]
ABSTRACT: Considering the growing use of steviol glycosides as natural sweetener and sugar substitute, there is an interest in efficient methods for the purification of individual steviol glycosides for example as reference compounds. In this work, we used countercurrent chromatography (CCC) for the isolation of several steviol glycosides from a stevia formulation. Gradient elution CCC with the two-phase solvent system ethyl acetate/n-butanol/water resulted in a higher separation efficiency than the classic isocratic elution mode. In this way, 1.7 mg of steviolbioside, 2.2 mg of dulcoside A, 5.7 mg of rebaudioside A, 4.1 mg of rebaudioside B and 1.2 mg rebaudioside D (purities >95 %) were obtained from the injection of 40.2 mg stevia formulation within 160 min. Purification of rebaudioside C (Reb C) and stevioside (St) was hampered by a similar partitioning behavior in the solvent system. The purity of the collected fractions containing steviol glycosides was assessed by HPLC and HPTLC and the structures were confirmed by HPTLC coupled to ESI–MS. A strong discrepancy between the theoretical maximum sample load (630 mg) and the experimental sample load (40 mg) was observed and surface-active properties of the steviol glycosides were found to be responsible for total stationary phase flooding which occurred in case of higher sample loads.
No preview · Article · Jan 2016 · Chromatographia
• ##### Article: Development of a Straightforward and Cheap Ethyl Acetate Based Method for the Simultaneous Determination of Pesticides and Veterinary Drugs Residues in Bovine Liver and Muscle
[Hide abstract]
ABSTRACT: The optimization and validation study of a qualitative and quantitative multiclass, ethyl acetate (EtOAc) multi-residue method to straightforward monitor 48 compounds in liver (6 veterinary drugs and 42 pesticides) and 54 in muscle (5 veterinary drugs and 49 pesticides) followed by high performance liquid chromatography tandem mass spectrometry (HPLC–MS/MS) and gas chromatography mass-spectrometry determination (GC–MS) is presented. Several clean-up sorbents were evaluated looking for the best strategy for the removal of the matrix co-extractives. A combination of aluminium oxide, (Al2O3), C-18 and magnesium sulphate (MgSO4) yielded the best analytical results in terms of precision and accuracy. The method was validated at three fortification levels: 10, 100 and 250 µg kg−1. The percentages of recovery were between 70 and 114 % for bovine muscle and 70–118 % for liver. Repeatability and intermediate precision percentages were below 20 % for both matrices. Most of the compounds under study presented good linearity and quantification limits below their corresponding European Union (EU) and Codex Alimentarius maximum residue levels (MRLs). Twenty-two randomly taken real samples were analyzed with the validated methodology, trying to prove its effectiveness and suitability for routine analysis. The validated methodology represents a fast and cheap alternative for the simultaneous analysis of pesticides and veterinary drugs which can be easily extend to other compounds and matrices.
No preview · Article · Jan 2016 · Chromatographia
• ##### Article: Case Study: Beehive Devastation by Microencapsulated Parathion-Methyl
[Hide abstract]
ABSTRACT: During spring 2012, massive honeybee mortality was observed within 2000 beehives in southwest Uruguay. The incident was presumed to be due to pesticide applications in the hives surroundings. To find the causative agent, bees were analyzed by gas and liquid chromatography coupled t o mass spectrometry, employing a method reported by our group that has been expanded to 39 compounds. The new scope includes parathion-methyl, which was found at an average 0.48 µg bee−1, ten times higher than the LD50 for bees. Parathion-methyl is only allowed to be sold as microcapsules, a slow release formulation type with 80–50 µm particle diameter. Surprisingly, it was stated that parathion-methyl microcapsules were applied in the zone but 1000–2000 m ahead from the affected hives. This fact was not only a confirmation of the distances bees can fly from the hive, but also demonstrated that the microcapsules, mistaken for pollen, were transported to the hive where the toxic was released. Although microcapsules have environmental advantages as a pesticide delivery system they can threaten honeybees’ survival.
No preview · Article · Jan 2016 · Chromatographia
• ##### Article: Surface Characteristics and Physicochemical Properties of Polystyrene-b-Poly(Acrylic Acid) Determined by Inverse Gas Chromatography
[Hide abstract]
ABSTRACT: Surface and bulk properties of polystyrene-b-poly(acrylic acid) (PS-b-PAA) were determined by inverse gas chromatography (IGC) technique. The determined surface properties were dispersive component of surface energy, $$\gamma_{\text{S}}^{\text{D}}$$, Lewis acid and base constants, $$K_{\text{A}}$$ and $$K_{\text{D}}$$, respectively. The dispersive component of surface energy ranged from 39.9 to 20.9 mJ m−2 at a temperature range from 303 to 343 K while $$K_{\text{A}}$$ and $$K_{\text{D}}$$ were found to be 0.083, and 0.781, respectively, at this temperature range. The higher $$K_{\text{D}}$$ than $$K_{\text{A}}$$ suggested the surface of the copolymer was basic. The bulk polymer interaction parameters such as weight fraction activity coefficient, $$\varOmega_{1}^{\infty }$$, Flory–Huggins interaction parameter, $$\chi_{12}^{\infty }$$, equation-of-state interaction parameter, $$\chi_{12}^{ * }$$, and effective exchange energy parameter, $$X_{\text{eff}}$$ of PS-b-PAA were determined using the retention data of several solvents at temperatures between 413 and 453 K.
No preview · Article · Jan 2016 · Chromatographia
• ##### Article: Alternative Liquid–Liquid Microextraction as Cleanup for Determination of Neonicotinoid Pesticides Prior HPLC Analysis
[Hide abstract]
ABSTRACT: A simple microextraction, namely low-density solvent with low-toxicity organic solvent-based dispersive liquid–liquid microextraction (LDS-DLLME) and modified QuEChERS sample preparation procedures were optimized and validated for preconcentration of neonicotinoid pesticides prior to the determination using HPLC. The experimental parameters affecting the extraction efficiency, including salt addition, type of disperser solvent and its volume, effect of extraction solvent and its volume, and extraction time were investigated. Under the selected LDS-DLLME and HPLC conditions, separation of seven neonicotinoid pesticides (imidacloprid, acetamiprid, clothianidin, thiacloprid, thiamethoxam, dinotefuran, and nitenpyram) was achieved within 26 min. 1-Octanol (extraction solvent) and acetonitrile (disperser solvent) were used for extraction of the target analytes. Under the optimum condition, linearity was obtained within the range of 0.1–1000 ng g−1 with a correlation coefficient more than 0.999. The high enrichment factor of the target analytes was 50-fold and a low limit of quantitation (0.80–2.50 ng g−1) could be obtained. The fruit samples (at fortified levels of 10, 30, and 50 ng g−1) were successfully analyzed, and relative recoveries were obtained in the range of 90.07–112.22 %.
No preview · Article · Jan 2016 · Chromatographia
• ##### Article: An On-Column Enzyme Mediated Fluorescence-Amplification Method for Plasma Total Cholesterol Measurement by Capillary Electrophoresis with LIF Detection
[Hide abstract]
ABSTRACT: Total cholesterol monitoring in human plasma is one of the most important routine analysis performed in the clinical laboratory. Here we report a new capillary electrophoresis method for determination of plasma total cholesterol based on on-column enzymatic assay and laser-induced fluorescence detection. In this method, the capillary is used not only as a separation medium but also as the reaction chamber which minimizes the amount of samples and the consumption of the reagents. The whole procedure can be automated which minimizes the possible errors and saves experimental time. The analytical characteristics of the proposed method, such as linearity and repeatability of the peak area and the migration time, were evaluated. The RSD of the migration time and peak area were 1.0 and 3.5 % (intraday), and 2.2 and 2.9 % (interday), respectively. The obtained LOQ values were at the nanomolar concentration level, therefore the developed method is sufficient for determination and quantification of plasma total cholesterol.
No preview · Article · Jan 2016 · Chromatographia
• ##### Article: Analyses of Nonsteroidal Anti-inflammatory Drugs in Human Plasma Using Dispersive Nano Solid-Phase Extraction and High-Performance Liquid Chromatography
[Hide abstract]
ABSTRACT: Iron nanoparticles were synthesized by green technology. These were functionalized with 1-butyl-3-methylimidazolium bromide (ionic liquid) to enhance specificity and selectivity. Fourier transform infrared spectroscopy, energy dispersive X-ray fluorescence, X-ray diffraction, scanning electron microscopy and transmission electron microscopy were used for characterization. 1-Butyl-3-methylimidazolium bromide-functionalized iron nanoparticles (BMIF-INPs) were applied in nano dispersive solid-phase extraction for the extraction of nonsteroidal anti-inflammatory drugs (NSAIDs) from the plasma prior. The different extraction parameters such as type and amount of sorbents, agitation time, pH, desorbing solvents, desorbing volume, and desorption times were optimized. Optimum conditions were 1.5 mg mL−1 of BMIF-INP sorbent, 20 min of agitation time, pH of 5.0, acetonitrile + 0.1 % acetic acid desorbing solvent, 600 µL of desorbing volume and 2 min of desorbing time. The percentage recoveries of all the six NSAIDs ranged from 87.4 to 94.98 %. High-performance liquid chromatography was developed using a pentafluorophenyl column (100 × 4.6 mm; 2.6 µm) and water–acetonitrile–acetic acid (70:30, v/v) of pH 3.0 with acetic acid as the mobile phase. The flow rate was 1.0 mL min−1 with detection at 240 nm. The values of k, α and R s ranged from 0.83 to 19.0, 1.16 to 6.13 and 1.0 to 5.76, respectively. The developed sample preparation and chromatographic methods were fast, selective, inexpensive, economical and reproducible. These methods have good applications and may be used for analyzing these drugs in biological, environmental and industrial matrices.
No preview · Article · Jan 2016 · Chromatographia
• ##### Article: Determination of Synthetic Food Colorants in Powder Beverage Samples by On-line HPLC–Cupric Reducing Antioxidant Capacity (CUPRAC) Assay with Post-Column Detection
[Hide abstract]
ABSTRACT: Due to the toxic and carcinogenic effects of some synthetic food colorants, their utilization is limited by food and health regulations. Synthetic colorants are preferred for their stability and low cost in food processing but their misuse may cause health hazards. The aim of this study is to determine food colorants by fast, accurate and applicable methods and inform consumers about the limitations of these substances. Thus, spectrophotometric CUPRAC (cupric ion reducing antioxidant capacity) assay was adapted for the determination of synthetic food colorants so as to define PECC (ponceau 4R equivalent colorant content) coefficients for the calculation of total colorant content of powder beverage samples. The PECC coefficients of the tested colorants were found in the following order: PECCerythrosine > PECCsunsetyellow > PECCtartrazine > PECCindigocarmine. HPLC and on-line HPLC derivatization techniques were developed for synthetic colorants. Total colorant content of synthetic and real (orange and rosehip powder beverage) samples were found and critically compared with the use of three methods, namely spectrophotometric CUPRAC, HPLC (with CUPRAC calculation) and on-line HPLC–post column CUPRAC assays. On-line HPLC–CUPRAC assay yielded low detection limits for colorants. Statistical analyses of the findings of these three methods using the two-way ANOVA test proved that the developed methods for determining synthetic food colorants are accurate, diversely applicable, and well-correlating.
No preview · Article · Jan 2016 · Chromatographia
• ##### Article: Comparison of Four Extraction Methods for the Determination of Veterinary Pharmaceuticals in Sediment
[Hide abstract]
ABSTRACT: In this work extraction by agitation (EA), ultrasound solvent extraction (USE), microwave assisted extraction (MAE) and pressurized liquid extraction (PLE) followed by high performance liquid chromatography with diode array detector (HPLC–DAD) for the determination of eight veterinary pharmaceuticals from different structural groups including one macrolide (tylosine), three anthelmintics (albendazole, febantel and levamisole), two anesthetics (lidocaine and procaine) and two steroidal hormones (hydrocortisone and dexamethasone) in sediment is described. Selected pharmaceuticals are widely used in veterinary practice in Croatia and in the whole world. Since they belong to different structure groups the usage of routine methods is not effective for their extraction from a complex sediment sample. Also, until now no article has been published for systematic extraction of named pharmaceuticals from sediment sample by different extraction methods. EA, USE, MAE and PLE have been optimized regarding different characteristic parameters such as sediment mass, extraction solvent, solvent volume, agitation frequency, power of ultrasound bath, extraction duration, extraction temperature and contact time between sediment and solvent. After extraction, pharmaceuticals were analyzed by HPLC–DAD using C18 stationary phase. HPLC–DAD–EA, HPLC-USE, HPLC–DAD-MAE and HPLC–DAD–PLE methods were validated in terms of selectivity, specificity, linearity, sensitivity, method detection limit (MDL) and quantification (MQL), repeatability, recovery and stability of a standard solution. Recoveries of selected pharmaceuticals from spiked sediment samples were generally higher than 50 %. However, dexamethasone and hydrocortisone showed lower recoveries due to their significantly different molecule structure. This paper shows the ability of simultaneous extraction and analysis of all selected pharmaceuticals by four different extraction methods in complex sediment sample followed by relatively affordable and sensitive HPLC–DAD method.
No preview · Article · Jan 2016 · Chromatographia
• ##### Article: Development of an HPLC-FLD Method for Determination of Rhodamine-123 in Caco-2 Cell-Based Permeability Studies
[Hide abstract]
ABSTRACT: P-glycoprotein (P-gp) overexpression and its efflux pump function have been associated with chemotherapy failure in many cancers. Many cytotoxic agents have been P-gp substrates. Thus, it was essential to develop a simple and validated method to determine the P-gp substrate in the presence of P-gp inhibitors. In this study, the HPLC-FLD method was developed combined with Caco-2 cell-based permeability studies. First, we developed the HPLC method to quantify Rhodamine-123 (Rho-123) in transport media. It was validated to be sensitive, precise, accurate, linear and specific. Then, the method was employed to determine the Rho-123 concentration in the presence or absence of two known P-gp inhibitors, verapamil and tetrandrine, in a Caco-2 transepithelial transport experiment. The results showed that the two P-gp inhibitors decreased the secretory and increased the absorptive transport of Rho-123. It illustrated that the HPLC-FLD method for determination of Rho-123 in the presence of two P-gp inhibitors in Caco-2 cell-based permeability studies was accurate and reliable.
No preview · Article · Jan 2016 · Chromatographia