In this study, a flow-injection analysis (FIA) system with UV-detection is described for the direct determination of Acemetacin, which is antiinflammatory-analgesic drug used for the treatment of rheumatic diseases. The best suitable carrier solvent system was found to be 2 mM NaOH prepared in ethanol :water (20:80, v/v). Using a flow-rate of 1,2 mL min -1 and wavelength of 280,8 nm, the linear response was obtained for Acemetacin in the range of 1,2×10 -5 ‒5,8×10 -5 M (5,0‒24,1 μg mL -1 ) with a detection limit of 1,6×10 -6 M (0,7 μg mL -1 ). The proposed method was successfully applied to the determination of Acemetacin in commercial capsules and results were compared by a simple UV-spectrophotometric method developed in this study.

In this study, a simple, efficient and rapid Ultra High Performance Liquid Chromatography method with fluorescence detection (UHPLC-FLD) has been developed and validated for the determination of Ochratoxin-A (OTA) in rat brain microdialysates and plasma samples. Six adult male wistar rats were used in the study and a single dose (5 mg/kg b.w.) of OTA was given by intraperitoneal (i.p.) injection. Rat blood and microdialysate samples were collected simultaneously after i.p. injection in awake freely moving rats, over a twelve-hour period. An UHPLC analysis was performed on a Zorbax Eclipse Plus C8 (150 mm × 3.0 mm ID × 1.8 μm particles) column with a mobile phase of acetonitrile:water:phosphoric acid (50:50:0.1, v/v) using a flow rate of 0.6 mL/min. The fluorescence detector was set at 330 nm excitation and 460 nm emission wavelengths. Diflunisal (DIF) was used as an internal standard (IS). OTA and IS were separated within 5 min under these conditions. The method was validated in terms of linearity, precision, accuracy, limit of detection, limit of quantification, and stability. Calibration curves obtained with spiked biological matrices show good linearity with high correlation coefficients. The intra- and inter-day assay variability was <5% for the OTA. The limit of detection and the limit of quantification values were found to be 0.490 ng/mL and 1.48 ng/mL for plasma; 0.0900 ng/mL and 0.270 ng/mL for microdialysate samples, respectively. This method was successfully applied for the monitoring of OTA levels in the rat brain and plasma samples.

A simple and validated micellar electrokinetic chromatographic method is described for the determination of 5-hydroxymethylfurfural (HMF). The method was applied to fresh and processed (heated at 65 °C, 85 °C and 105 °C for 5 h and 20 h) multifloral and honeydew honeys. Optimum conditions were: 10 mmol L−1 Tris buffer consisting 110 mmol L−1 SDS and 10% (v/v) MeOH at pH 9.10, 20 kV of applied potential, 3 s of injection time at 5 × 103 N m−2, 280 nm of wavelength and 25 °C of fixed temperature. Mean electrophoretic mobility (m2 s−1 V−1) of HMF and methyl paraben (IS) were − 5.28 × 10−5 (RSD of 0.745%) and − 2.52 × 10−4 (RSD of 0.944%), respectively. The calibration curve was linear in the range of 0.68 µg mL−1 (5.40 × 10−6 mol L−1) and 4.05 µg mL−1 (3.21 × 10−5 mol L−1) with R = 0.9990 for inter-day precision. LOD and LOQ values were 0.007 µg mL−1 (5.48 × 10−8 mol L−1) and 0.023 µg mL−1 (1.83 × 10−7 mol L−1), respectively, as inter-day precision. The accuracy was very high with recovery values between 94.07 and 97.16%. The developed method was fully validated according to ICH guidelines. The results were compared with those of HPLC method adapted from AOAC method no: 980.23.

Bu çalışmada romatizma tedavisinde kullanılan antiinflamatuvar-analjezik etkili ilaçlardan Asemetasin bileşiğinin doğrudan tayininde UV-dedektörlü akış-enjeksiyon analiz (FIA) tekniği tanımlanmıştır. En uygun taşıyıcı çözücünün, etanol:su (20:80, h/h) içerisinde hazırlanan 2 mM NaOH olduğu saptanmıştır. Akış hızı olarak 1,2 mL dak-1 ve çalışma dalga boyu olarak 280,8 nm değerleri kullanıldığında Asemetasin için 1,2×10-5‒5,8×10-5 M (5,0‒24,1 μg mL-1)derişim aralığında, 1,6×10-6 M (0,7 μg mL-1) gözlenebilirlik sınırına sahip doğrusal bir aralık elde edilmiştir. Önerilen yöntem, bu bileşiği içeren ticari kapsül ilaç şekline başarıyla uygulanmış ve sonuçlar bu çalışmada geliştirilen basit bir UV-spektrofotometrik yöntemle karşılaştırılmıştır.

A validated rapid and sensitive capillary zone electrophoretic method for the determination of olopatadine hydrochloride (OLO) is described. Optimum conditions were found: 20 mmol/L sodium tetraborate buffer, acetonitrile 15% (v/v), 10 mmol/L NaCl at pH 9.5, with 25 kV of applied potential, injection time of 10 s at 5 × 103 N/m2, at a wavelength of 205 nm, and fixed temperature of 30°C. The calibration curve was linear in the range of 1.13 × 10-5 mol/L (4.22 μg/mL) to 5.65 × 10-5 mol/L (21.12 μg/mL), with R = 0.9995 for interday precision. LOD and LOQ values were 1.58 × 10-6 (0.58 μg/mL) and 4.78 × 10-6 mol/L (1.75 μg/mL), respectively. Precision values were 1.10-1.97% for intraday and 1.41% for interday RSDs. Accuracy was tested by preparing a synthetic mixture whose composition was similar to the pharmaceutical preparation for Patanol. The RSDs of the recovery values (98.2%) were between 0.42 and 0.65% and the amount of OLO found was 1.09 mg/mL. The result was within the requirements of USP 31-NF 26. Therefore, this validated method is suggested for routine analysis for the determination of OLO in laboratories.

This article presents a newly developed capillary gel electrophoresis (CGE) using dynamic coating with hydroxyethylcellulose methodology for the separation of fourteen standard DNA fragments and determination of RAPD-PCR products after a PCR purification clean-up procedure for certain Salvia (sage) species. The developed CGE was successfully applied to the RAPD products of ten different Turkish Salvia (sage) species (Salvia bracteata, S. candidissima, S. ceratophylla, S. dichroantha (endemic), S. forskahlei, S. fruticosa, S. sclarea, S. tomentosa, S. verticillata, and S. viridis). These medicinal plants exhibit a wide range of Turkish flora. The CGE results were compared with those by the slab gel electrophoresis (SGE). The present study offers an alternative CGE method to SGE for the effective separation and evaluation of RAPD-PCR products. This CGE has certain advantages to SGE on the viewpoint of requiring smaller amount of sample and solvent, higher resolution and speed, easier automation, higher sensitivity, and online detection. DNA analysis in Salvia species can help further understanding of their biological functions. In this study, a phylogenetic relationship was analysed by SGE. S. fruticosa and S. dichroantha are genetically the most distant species, and S. bracteata and S. fruticosa are the the most similar species.Keywords: capillary gel electrophoresisDNAphylogenetic treeRAPD-PCRSalviaslab gel electrophoresis AcknowledgmentsThis article was derived from the PhD thesis of Elif Mine Öncü-Kaya.[Citation53] The authors are grateful to Onur Koyuncu, Ömer Koray Yaylacı, and İlham Eröz Poyraz for the collection and identification of the Salvia species. We also appreciate the proofreading of the paper carried out by Edward McQuaid, an English teacher at Anadolu University.

A validated liquid chromatography method employing a fluorescence detector for the determination of ochratoxin A (OTA) was developed with double internal standard and it was applied to ten different poultry feeds. The analysis was performed in an octadecyl silane column using a solvent system [ACN:water:formic acid (50:50:1.25, v/v/v)] by isocratic elution. The flow rate and injection volume were 1 mL min^{-1} and 12 \mu L, respectively. Signals were detected at 278(\lambda_{ex})/315(\lambda_{em}) and 330(\lambda_{ex})/450(\lambda_{em}) nm between 0 and 8, and 8.01 and 20.0 min, respectively. The method was validated with precision, linearity, accuracy, limit of detection, limit of quantification, robustness, and stability. Good linearity (r^2 = 0.9998--0.9999) was achieved over a concentration range of 1.60 \times 10^{-8} M to 6.40 \times 10^{-6} M for OTA. LOD and LOQ values were 7.83 \times 10^{-10} M and 2.37 \times 10^{-9} M, and 2.01 \times 10^{-9} M and 6.10 \times 10^{-9} M for internal standard 1 (IS1) and internal standard 2 (IS2), respectively, on an interday basis. The method was applied to poultry feed samples. Good recovery data ranged between 79.10% and 85.57%, and 71.98% and 76.66%, and the RSD% values were in the range of 1.36--11.70 and 2.07--2.34 for IS1 and IS2, respectively.

This article presents a newly developed capillary gel electrophoresis (CGE) using dynamic coating with hydroxyethylcellulose methodology for the separation of fourteen standard DNA fragments and determination of RAPD-PCR products after a PCR purification clean-up procedure for certain Salvia (sage) species. The developed CGE was successfully applied to the RAPD products of ten different Turkish Salvia (sage) species (Salvia bracteata, S. candidissima, S. ceratophylla, S. dichroantha (endemic), S. forskahlei, S. fruticosa, S. sclarea, S. tomentosa, S. verticillata, and S. viridis). These medicinal plants exhibit a wide range of Turkish flora. The CGE results were compared with those by the slab gel electrophoresis (SGE). The present study offers an alternative CGE method to SGE for the effective separation and evaluation of RAPD-PCR products. This CGE has certain advantages to SGE on the viewpoint of requiring smaller amount of sample and solvent, higher resolution and speed, easier automation, higher sensitivity, and online detection. DNA analysis in Salvia species can help further understanding of their biological functions. In this study, a phylogenetic relationship was analysed by SGE. S. fruticosa and S. dichroantha are genetically the most distant species, and S. bracteata and S. fruticosa are the the most similar species.

Bu calisma, bebek mamalarinin paketin acildigi birinci ve onbesinci gunlerdeki d-pantotenat ve niasinin degisiminin yeni bir kapiler elektroforetik yontemle zamana bagimli olarak degisimini tanitmaktadir. Se­kiz numunede D-pantotenat miktari Turk Standartlarinin belirledigi degerlerden yuksek bulunmus, dokuz numunede bulunmamistir. Yedi numunede niasine rastlanmamistir. On besinci gunde tum numunelerde vitamin kayibi gozlenmistir.

A capillary zone electrophoretic method for the determination of zearalenone is described in this study. In the separation, a run buffer consisting of 20mM sodium tetraborate at pH 9.0 with 15% acetonitrile applying 15kV, injecting 10s at 50 mbar was utilized. Phenobarbital was a suitable internal standard and the signals were recorded at 254nm. Zearalanon and internal standard appeared at 5.46min (RSD% 0.20) and 6.35min (RSD% 0.18), respectively. The repeatability results are in the range of 0.011.58 for inter-day. The linearity was investigated in the range of 5.20x107M to 7.86x105M ZEA and it was linear fitting to the equation of [rPN=244803.8 C(M) 0.0348; r=0.9999]. The LOD and LOQ were calculated to be 2.70x108M (8.25 mu g/L) and 8.17x108M (25 mu g/L), respectively. Then, the method was successfully applied to the analysis of ZEA in poultry feeds, flour of maize, grain, and certain cereal samples such as fibrous biscuit, popcorn, and rice crisp.

A capillary zone electrophoretic method for the determination of zearalenone is described in this study. In the separation, a run buffer consisting of 20 mM sodium tetraborate at pH 9.0 with 15% acetonitrile applying 15 kV, injecting 10 s at 50 mbar was utilized. Phenobarbital was a suitable internal standard and the signals were recorded at 254 nm. Zearalanon and internal standard appeared at 5.46 min (RSD% 0.20) and 6.35 min (RSD% 0.18), respectively. The repeatability results are in the range of 0.01–1.58 for inter-day. The linearity was investigated in the range of 5.20 × 10−7 M to 7.86 × 10−5 M ZEA and it was linear fitting to the equation of [rPN = 244803.8 C(M) −0.0348; r = 0.9999]. The LOD and LOQ were calculated to be 2.70 × 10−8 M (8.25 µg/L) and 8.17 × 10−8 M (25 µg/L), respectively. Then, the method was successfully applied to the analysis of ZEA in poultry feeds, flour of maize, grain, and certain cereal samples such as fibrous biscuit, popcorn, and rice crisp.

A novel precolumn derivatization reversed-phase high-performance liquid chromatography method with fluorescence detection is described for the determination of ranitidine in human plasma. The method was based on the reaction of ranitidine with 4-fluoro-7-nitrobenzo-2-oxa-1,3-diazole forming yellow colored fluorescent product. The separation was achieved on a C(18) column using methanol-water (60:40, v/v) mobile phase. Fluorescence detection was used at the excitation and emission of 458 and 521 nm, respectively. Lisinopril was utilized as an internal standard. The flow rate was 1.2 mL/min. Ranitidine and lisinopril appeared at 3.24 and 2.25 min, respectively. The method was validated for system suitability, precision, accuracy, linearity, limit of detection, limit of quantification, recovery and robustness. Intra- and inter-day precisions of the assays were in the range of 0.01-0.44%. The assay was linear over the concentration range of 50-2000 ng/mL. The mean recovery was determined to be 96.40 ± 0.02%. This method was successfully applied to a pharmacokinetic study after oral administration of a dose (150 mg) of ranitidine.

This study describes a capillary zone electrophoretic method for the determination of patulin. An optimum run buffer was found to be 25 mM of sodium tetraborate and 10% acetonitrile (v/v) at pH 10. Optimum conditions were determined to be: an applied voltage of 25 kV (normal polarity), temperature of 25°C and injection time of 10 s at 50 mbar; the signals of patulin and phenobarbital as internal standard were detected at 276 nm. The method was highly reproducible, with relative standard deviations of 0.02-0.85 for intra-day and 0.04-0.42 for inter-day for standard patulin. Acceptable linearity [y = 0.0020C (μg/L) - 0.0680 (r = 0.9999)] was obtained over a concentration range of 0.25 to 4.99 µg/mL of patulin. The limits of detection and quantification were calculated to be 5.9 × 10(-3) and 1.79 × 10(-2) µg/mL, respectively. Recovery was 68.0%. The proposed method was applied to 21 apple juice samples purchased from different Turkish markets, and two were found to contain higher than the limits of the European Union Directive for patulin.

A novel pre-column derivatization reversed-phase high-performance liquid chromatography with fluorescence detection is described for the determination of bupropion in pharmaceutical preparation, human plasma and human urine using mexiletine as internal standard. The proposed method is based on the reaction of 4-chloro-7-nitrobenzofurazan (NBD-Cl) with bupropion to produce a fluorescent derivative. The derivative formed is monitored on a C18 (150 mm × 4.6 mm i.d., 5 µm) column using a mobile phase consisting of methanol-water 75:25 (v/v), at a flow-rate of 1.2 mL/min and detected fluorimetrically at λ(ex) = 458 and λ(em) = 533 nm. The assay was linear over the concentration ranges of 5-500 and 10-500 ng/mL for plasma and urine, respectively. The limits of detection and quantification were calculated to be 0.24 and 0.72 ng/mL for plasma and urine, respectively (inter-day results). The recoveries obtained for plasma and urine were 97.12% ± 0.45 and 96.00% ± 0.45, respectively. The method presents good performance in terms of precision, accuracy, specificity, linearity, detection and quantification limits and robustness. The proposed method is applied to determine bupropion in commercially available tablets. The results were compared with an ultraviolet spectrophotometry method using t- and F-tests.

The infusions and extracts obtained from leaves with flowers, fruit peel, and seed from hawthorn (Crataegus monogyna Jacq., Family Rosaceae) were subjected to evaluation as potential sources of antioxidant phytochemicals on the basis of their total content of phenolics, levels of phenolic acids, and in vitro antiradical activity. Total phenolic content of extracts was determined using the modified Folin-Ciocalteau method. Antioxidant activity was determined for phenolic extracts by a method involving the use of the free radical 2,2-diphenyl-1-picrylhydrazyl (DPPH). Phenolic acids containing extracts and infusions from hawthorn leaves, fruit peel, and seeds were obtained using different polarity solvents and separated by reverse-phase high-performance liquid chromatography, which enabled improved separation by the use of a C(18) column, an acidic mobile phase, and gradient elusion. The highest total phenolic content (343.54 mg of gallic acid equivalents/g) and the highest DPPH radical scavenging activity as the inhibition percentage (60.36%) were obtained in ethyl acetate extract from hawthorn leaves with flower. Also, the highest phenolic acid content was measured in the extracts of hawthorn leaves with flowers: protocathechuic (108-128 mg/100 g), p-hydroxy benzoic (141-468 mg/100 g), caffeic (137-3,580 mg/100 g), chlorogenic (925-4,637 mg/100 g), ferulic (3,363-3,462 mg/100 g), vanillic (214 mg/100 g), and syringic (126 mg/100 g) acids. The results indicate that hawthorn is a promising plant because of its high antioxidant activity.

A new high performance liquid chromatography (HPLC) method was developed based on an indirect determination of tannase activity through gallic acid measurement using paracetamol as an internal standard. The separation was performed on a C(18) column using a mobile phase consisting of aqueous formic acid solution (1%) and methanol (85:15; v/v) pumped at 1 ml min(-1). Samples (10 mu l) were injected and signals were detected at 254 nm. Repeatability was 0.81 and 1.28 for peak normalization values of gallic acid (4.16 x 10(-5) M) and internal standard (2.02 x 10(-5) M). A good linearity was shown in the range of 1.04 x 10(-5) to 8.32 x 10(-5) M. Limit of detection (LOD) and limit of quantification (LOQ) values were calculated to be 2.2 x 10(-6) M and 6.6 x 10(-6) M, respectively. The applicability of the method was tested using Penicillium spinulosum which produces tannase. The method was highly sensitive, accurate, reliable, and repeatable and at the same time it is applicable to both pure and crude enzyme.

This study describes the analysis of baby foods regarding time-dependent changes of d-pantothenate and niacin by a new capillary electrophoretic method at first and fifteenth days of opening the packages. Dpantothenate amounts in eight of the samples were found to be higher than those identified in the Turkish Standard and it was not detected in the nine samples. Niacin was not detected in the seven samples. Losses of mentioned vitamins were observed at the fifteenth-day for all samples

A simple extraction and determination method for folic acid (FA) in lentil samples was developed employing capillary electrophoresis. The analysis was performed in a 75 μm ID fused silica capillary using a running buffer of 10 mM sodium borate (10%, v/v, methanol, pH 9) at +18 kV and a detection wavelength at 200 nm. Methylparaben was used as the internal standard. FA signal response was linear in the range between 1.2 × 10−5 and 4.8 × 10−5 M. Limit of detection (inter-day) was determined at 6.12 × 10−7 M (3.3 σs−1). The amount of FA found in green, red and mignon lentils was found to range between 0.408 and 0.742 mg g−1.

Due to being one of the most important dietary staple foods in the world, corn (Zea mays) has gained considerable attention. Drying is an essential procedure for safe storage of corn. The objectives of the present study were to investigate the effects of infrared (IR), hot air (HA) and infrared-hot air combined (IR-HA) drying on some properties of corn and to offer an alternative drying procedure with low energy costs. Crude protein, total carotenoid, phenolic acid composition, color parameters (L, a+, b+, chroma, Hue angle, Delta E) and energy expenses of the drying techniques in terms of specific energy consumption (SEC) for unit evaporated water were evaluated. Dent corn samples were hand harvested at regular intervals of fortnight at maturity and the initial moisture contents were 24, 16 and 15%, respectively. Preparation was included kernel manual trimming and granulating. Kernels were dried until the moisture content comes down to 13% with IR, HA and IR-HA combination techniques except for control. All drying treatments were conducted at 45 degrees C. It was observed that IR radiation did not cause any negative impact on the stated properties of corn in noted conditions. Besides, IR and IR-HA drying methods dramatically reduced the drying time. Specific energy consumption values showed that IR and IR-HA combined systems are more effective and economic when the initial moisture content of corn is above 16%. Evaporation of unit water took 12 and 40% less energy in IR drying of corn samples with the initial moisture content of 24 and 16%, respectively, as compared to HA drying alone. Hence, IR drying is considered to be a promising alternative for corn drying.

This study describes a method development for the determination of rosmarinic acid (RA) by using a gradient high-performance liquid chromatography (HPLC) and its application to certain plant materials. The analysis was performed by utilizing a two solvents system [ A : methanol/water/formic acid (10:88:2; v : v : v ); B : methanol/water/formic acid (90:8:2; v : v : v )] on a reverse-phase column. The flow rate and injection volume were 1 ml min −1 and 10 μl, respectively. Signals were detected at 280 nm. In addition, an internal standard (IS) technique was applied for the analysis of RA to increase precision, and propylparaben was employed for this purpose. The repeatability results as RSD% were 1.66, 1.17 and 1.26 for intra-day and 1.38 was for inter-day with the employment of (3.67 × 10 −5 M) RA. A limit of linearity (LOL) was observed in a wide (1.13 × 10 −5 –5.65 × 10 −4 M) concentration range. Linearity parameters were also examined in the range of 5.95 × 10 −6 –7.14 × 10 −5 M RA, and very good correlation was observed. The limit of detection (LOD) and limit of quantification (LOQ) (for inter-day) were 1.60 × 10 −6 M (signal/noise [S/N] = 3.3) and 4.80 × 10 −6 M (S/N = 10), respectively. The method was applied to the extracts of certain Lamiaceae plants ( Salvia candidissima Vahl. subsp. candidissima, S. sclarea L., S. verticillata L. subsp. v erticillata and R. officinalis L.), and reasonable results were obtained.