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Analytical Laboratories (analytical + laboratory)
Selected AbstractsMulti-laboratory validation of a standard method for quantifying proanthocyanidins in cranberry powdersJOURNAL OF THE SCIENCE OF FOOD AND AGRICULTURE, Issue 9 2010Ronald L Prior Abstract BACKGROUND: The objective of this study was to validate an improved 4-dimethylaminocinnamaldehyde (DMAC) colorimetric method using a commercially available standard (procyanidin A2), for the standard method for quantification of proanthocyanidins (PACs) in cranberry powders, in order to establish dosage guidelines for the uropathogenic bacterial anti-adhesion effect of cranberry. RESULTS: Commercially available cranberry samples were obtained (five from U.S. sources and six from European sources) for PAC quantification in five different analytical laboratories. Each laboratory extracted and analyzed the samples using the improved DMAC method. Within-laboratory variation (mean ± SD) was 4.1 ± 1.7% RSD (range, 2.3,6.1% RSD) and the between laboratory variability was 16.9 ± 8.5% RSD (range, 8,32% RSD). For comparative purposes, the cranberry samples were alternatively quantified using weights of extracted PACs (gravimetric). The correlation coefficient between the two methods was 0.989. CONCLUSION: This improved DMAC method provides a simple, robust and relatively specific spectrophotometric assay for total PACs in cranberry samples using commercially available procyanidin A2 dimer as a standard. DMAC is most useful within a given type of food such as cranberries, but may not be appropriate for comparing concentrations across different food types, particularly in those cases where large differences exist among the relative amounts of each oligomer and polymer. Copyright © 2010 Society of Chemical Industry [source] Comparison of triple quadrupole, hybrid linear ion trap triple quadrupole, time-of-flight and LTQ-Orbitrap mass spectrometers in drug discovery phase metabolite screening and identification in vitro , amitriptyline and verapamil as model compoundsRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 7 2010Timo Rousu Liquid chromatography in combination with mass spectrometry (LC/MS) is a superior analytical technique for metabolite profiling and identification studies performed in drug discovery and development laboratories. In the early phase of drug discovery the analytical approach should be both time- and cost-effective, thus providing as much data as possible with only one visit to the laboratory, without the need for further experiments. Recent developments in mass spectrometers have created a situation where many different mass spectrometers are available for the task, each with their specific strengths and drawbacks. We compared the metabolite screening properties of four main types of mass spectrometers used in analytical laboratories, considering both the ability to detect the metabolites and provide structural information, as well as the issues related to time consumption in laboratory and thereafter in data processing. Human liver microsomal incubations with amitriptyline and verapamil were used as test samples, and early-phase ,one lab visit only' approaches were used with all instruments. In total, 28 amitriptyline and 69 verapamil metabolites were found and tentatively identified. Time-of-flight mass spectrometry (TOFMS) was the only approach detecting all of them, shown to be the most suitable instrument for elucidating as comprehensive metabolite profile as possible leading also to lowest overall time consumption together with the LTQ-Orbitrap approach. The latter however suffered from lower detection sensitivity and false negatives, and due to slow data acquisition rate required slower chromatography. Approaches with triple quadrupole mass spectrometry (QqQ) and hybrid linear ion trap triple quadrupole mass spectrometry (Q-Trap) provided the highest amount of fragment ion data for structural elucidation, but, in addition to being unable to produce very high-important accurate mass data, they suffered from many false negatives, and especially with the QqQ, from very high overall time consumption. Copyright © 2010 John Wiley & Sons, Ltd. [source] Determination of terbinafine hydrochloride in cat hair by two chromatographic methodsBIOMEDICAL CHROMATOGRAPHY, Issue 8 2001Jernej Kuz Terbinafine hydrochloride (terbHCl) concentration on the site of infection with Microsporum canis is a very important indicator of drug effectiveness. Several chromatographic methods exist that can be used for the determination of terbHCl concentration in biological samples. A high performance liquid chromatographic (HPLC) method and a gas chromatographic (GC) method have been compared and critically evaluated for the determination of a terbHCl levels in cat hair. The sensitivity and the linearity of the previously developed HPLC method were 0.25,ng/mL and 0.25,3000,ng/mL, respectively. The limit of quantification (LOQ) was 0.01,µg/g of terbHCl in cat hair, and reproducibility of 96.6% and recovery of 93.8% were achieved using appropriate sample pre-treatment and optimal chromatographic conditions. The sensitivity of the GC method, 25,ng/mL (LOQ 625 ppb), was much lower than that of the HPLC method. The GC method still enables determination of terbHCl in a range of concentrations in cat hair. The reproducibility of terbHCl for the cat hair samples was 95.3% and the recovery was only 70.0%. Both methods can be used for the evaluation of drug effectiveness in cats and both of them require only basic chromatographic equipment that can be found in most analytical laboratories. Copyright © 2001 John Wiley & Sons, Ltd. [source] Linking data to electronic recordsQUALITY ASSURANCE JOURNAL, Issue 2 2003Heather Longden Abstract Today it is possible to maintain electronic records in a single application in compliance with 21 CFR Part 11. However, most electronic data for a sample in an analytical laboratory is spread across a number of software applications as well as traditional paper systems. This article will examine how it is possible to link both paper and electronic records together in hybrid systems. A case study is used to demonstrate the practical aspects of a totally electronic process. Copyright © 2003 John Wiley & Sons, Ltd. [source] Photostability studies for micellar liquid chromatographic determination of nifedipine in serum and urine samplesBIOMEDICAL CHROMATOGRAPHY, Issue 2 2006M. T. Gil-Agustí Abstract Nifedipine is a photosensitive compound that is converted into its 4-(2-nitrophenyl) pyridine and 4-(2-nitrosophenyl) pyridine homologue. In order to obtain the most adequate conditions for handling nifedipine solutions in the analytical laboratory, a number of studies on the decomposition of this compound were performed. A simple micellar liquid chromatographic procedure was described to determine nifedipine in different biological matrices such as serum and urine, and to control its decomposition. To perform the analysis, nifedipine was dissolved in 0.1 m SDS at pH 3 and chromatographed using a mobile phase containing 0.125 m SDS,3% pentanol, pH 3 on a C18 column and UV detection at 235 nm. The chromatographic analysis time was 8 min. The response of the drug for both biological matrices was linear in the 1,100 µg/mL range, with r2 > 0.997 at all times. Repeatability, intermediate precision (CV, %) and limits of quantification and detection (ng/mL) were 0.19, 4.3, 104 and 31 in serum and 0.81, 2.1, 136 and 41 in urine. The method developed here does not show interferences or matrix effects produced by endogenous compounds. Micellar media and mobile phases have the advantage of stabilising the compounds, thus preventing photodegradation and allowing the direct injection of biological samples. Copyright © 2005 John Wiley & Sons, Ltd. [source] Continuous capillary electrophoresis with ,ow injection and its application for determination of Ephedrine and Pseudo-ephedrine in Chinese medicinal preparationsBIOMEDICAL CHROMATOGRAPHY, Issue 8 2004Zhongwei Pan Abstract This article presents a new, simple and rapid continuous separation method by combination of ,ow injection with capillary electrophoresis designed for the analysis of basic traditional Chinese medicines. The device was produced using commercial capillary and components readily available in analytical laboratory. In double-T con,guration, the designed horizontal separation channel was 25 µm i.d. × 146 mm length (an effective separation length of 93 mm) quartz capillary, with two vertical elicitation arms produced from 0.5 mm i.d. pump tubing. The capillary was embedded in a 40 × 20 × 3 mm organic glass base. Using the double-T con,guration, continuous introduction of a series of samples was achieved. More than 3.00 resolution for ephedrine and pseudo-ephedrine were obtained using 100 mm borate buffer (pH 9.80) within 8 min in 25 µm separation channel with an electrical ,eld strength of 137 V/cm (UV detection at 215 nm). The linear calibration range was 50,1500 µg/mL (ephedrine, r = 0.9982; pseudo-ephedrine, r = 0.9990) for both analytes. The limits of detection were 2.65 µg/mL for ephedrine and 2.92 µg/mL for pseudo-ephedrine. In this device, the contents of ephedrine and pseudo-ephedrine in ,ve Chinese medicinal preparations were determined with RSDs (n = 5) in range 1.16,4.51% and recoveries in range 90.4,114.6%. Copyright © 2004 John Wiley & Sons, Ltd. [source] | ||||||||||