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Selected papers from the latest issue:
Rapid characterization of caged xanthones in the resin ofGarcinia hanburyiusing multiple mass spectrometric scanning modes: the importance of biosynthetic knowledge based prediction
07 November 2011, 22:04:47
Publication year: 2011
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 6 November 2011
Jing Yang, Li Ding, Linlin Hu, Shaohong Jin, Wenyuan Liu, ...
Although the anticancer activities of the resin ofGarcinia hanburyihave been well demonstrated, the chemical composition of this medicinal plant is still not fully understood. In this study, a highly effective qualitative method was developed for rapidly profiling the target and non-target caged xanthones in the resin ofG. hanburyi. This method mainly involves three steps as follows: (1) Prediction of the possible unknown caged xanthones in the resin ofG. hanburyiaccording to the structure characters of the known ones and some well established biosynthetic knowledge; (2) Structure classification according to the diagnostic fragment ions (DFIs) of the known cagedGarciniaxanthones; (3) Detection and characterization of the target and non-target caged xanthones in the resin ofG. hanburyiusing multiple mass spectrometric (MS) scanning modes. By use of such procedures, mass spectrometric data can be used for confirming the rationally predicted chemical structure rather than sophisticated and time-consumed de novo structure elucidation of a completely unknown component. Finally, a total of 34 caged xanthones including 18 likely new ones from the resin ofG. hanburyiwere rapidly detected and characterized within one working day.
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 6 November 2011
Jing Yang, Li Ding, Linlin Hu, Shaohong Jin, Wenyuan Liu, ...
Although the anticancer activities of the resin ofGarcinia hanburyihave been well demonstrated, the chemical composition of this medicinal plant is still not fully understood. In this study, a highly effective qualitative method was developed for rapidly profiling the target and non-target caged xanthones in the resin ofG. hanburyi. This method mainly involves three steps as follows: (1) Prediction of the possible unknown caged xanthones in the resin ofG. hanburyiaccording to the structure characters of the known ones and some well established biosynthetic knowledge; (2) Structure classification according to the diagnostic fragment ions (DFIs) of the known cagedGarciniaxanthones; (3) Detection and characterization of the target and non-target caged xanthones in the resin ofG. hanburyiusing multiple mass spectrometric (MS) scanning modes. By use of such procedures, mass spectrometric data can be used for confirming the rationally predicted chemical structure rather than sophisticated and time-consumed de novo structure elucidation of a completely unknown component. Finally, a total of 34 caged xanthones including 18 likely new ones from the resin ofG. hanburyiwere rapidly detected and characterized within one working day.
Highlights
► A highly effective qualitative method for chemically profiling the resin ofGarcinia hanburyi. ► A total of 34 cagedGarciniaxanthones were rapidly characterized within one working day. ► A combination of biosynthetic knowledge guided prediction and LC-MS/MS is a promising protocol for rapidly profiling natural productsCloud point extraction combined with graphite furnace atomic absorption spectrometry for speciation of Cr(III) in human serum samples
07 November 2011, 22:04:47
Publication year: 2011
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 6 November 2011
Mei Sun, Qianghua Wu
A cloud point extraction(CPE) method for the preconcentration of ultra-trace chromium speciation in human serum samples prior to determination by graphite furnace atomic absorption spectrometry (GFAAS) had been developed in this paper. In this method, Cr(III) reacts with 1-(2-pyridylazo) -2-Naphthol(PAN) yielding a hydrophobic complex, which then is entrapped in the surfactant-rich phase, whereas Cr(VI) is remained in aqueous phase. Thus, separation of Cr(III) and Cr(VI) could be realized. Total chromium was determined after the reduction of Cr(VI) to Cr(III) by using ascorbic acid as reducing reagent. PAN was used not only as chelating reagent in CPE, but also as chemical modifier in GFAAS. Triton X-114 non-ionic surfactant had been used as an extraction medium. The main factors affecting CPE efficiency, such as pH of solution, concentration and kind of complexing agent, concentration of non-ionic surfactant, equilibration temperature and time, were investigated in detail. An enrichment factor of 83.5 was obtained for the preconcentration of Cr(III) with 10 mL solution. Under the optimal conditions, the detection limit of Cr(III) was 0.02 μg·L. The relative standard deviation was 2.6% for intra-day assay precision (n = 7,c= 10ng·mL), values of revovery for chromium were from 92.0% to 94.7% for three samples. This method is simple, accurate, sensitive and can be applied to determine ultra-trace chromium speciation in human serum.
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 6 November 2011
Mei Sun, Qianghua Wu
A cloud point extraction(CPE) method for the preconcentration of ultra-trace chromium speciation in human serum samples prior to determination by graphite furnace atomic absorption spectrometry (GFAAS) had been developed in this paper. In this method, Cr(III) reacts with 1-(2-pyridylazo) -2-Naphthol(PAN) yielding a hydrophobic complex, which then is entrapped in the surfactant-rich phase, whereas Cr(VI) is remained in aqueous phase. Thus, separation of Cr(III) and Cr(VI) could be realized. Total chromium was determined after the reduction of Cr(VI) to Cr(III) by using ascorbic acid as reducing reagent. PAN was used not only as chelating reagent in CPE, but also as chemical modifier in GFAAS. Triton X-114 non-ionic surfactant had been used as an extraction medium. The main factors affecting CPE efficiency, such as pH of solution, concentration and kind of complexing agent, concentration of non-ionic surfactant, equilibration temperature and time, were investigated in detail. An enrichment factor of 83.5 was obtained for the preconcentration of Cr(III) with 10 mL solution. Under the optimal conditions, the detection limit of Cr(III) was 0.02 μg·L. The relative standard deviation was 2.6% for intra-day assay precision (n = 7,c= 10ng·mL), values of revovery for chromium were from 92.0% to 94.7% for three samples. This method is simple, accurate, sensitive and can be applied to determine ultra-trace chromium speciation in human serum.
Highlights
► It is a new analytical method about ultra-trace chromium speciation in human serum samples. ► It is an new method for glycuresis diagnose in clinical. ► New complexing agent PAN for Cr(III) has been used in micellar system.Quantification of potential impurities by a stability indicating UV–HPLC method in niacinamide active pharmaceutical ingredient
07 November 2011, 22:04:47
Publication year: 2011
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 6 November 2011
Saji Thomas, Amber Bharati, Kalsang Tharpa, Ashutosh Agarwal
A sensitive, stability indicating reverse phase UV–HPLC method has been developed for the quantitative determination of potential impurities of niacinamide active pharmaceutical ingredient. Efficient chromatographic separation was achieved on C18 stationary phase in isocratic mode using simple mobile phase. Forced degradation study confirmed that the newly developed method was specific and selective to the degradation products. Major degradation of the drug substance was found to occur under oxidative stress conditions to form niacinamideN-oxide. The method was validated according to ICH guidelines with respect to specificity, precision, linearity and accuracy. Regression analysis showed correlation coefficient value greater than 0.999 for niacinamide and its six impurities. Detection limit of impurities was in the range of 0.003% to 0.005% indicating the high sensitivity of the newly developed method. Accuracy of the method was established based on the recovery obtained between 93.3% to 113.3% for all impurities.
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 6 November 2011
Saji Thomas, Amber Bharati, Kalsang Tharpa, Ashutosh Agarwal
A sensitive, stability indicating reverse phase UV–HPLC method has been developed for the quantitative determination of potential impurities of niacinamide active pharmaceutical ingredient. Efficient chromatographic separation was achieved on C18 stationary phase in isocratic mode using simple mobile phase. Forced degradation study confirmed that the newly developed method was specific and selective to the degradation products. Major degradation of the drug substance was found to occur under oxidative stress conditions to form niacinamideN-oxide. The method was validated according to ICH guidelines with respect to specificity, precision, linearity and accuracy. Regression analysis showed correlation coefficient value greater than 0.999 for niacinamide and its six impurities. Detection limit of impurities was in the range of 0.003% to 0.005% indicating the high sensitivity of the newly developed method. Accuracy of the method was established based on the recovery obtained between 93.3% to 113.3% for all impurities.
Highlights
► First report on quantitative determination of potential impurities of niacinamide ► The newly developed HPLC method was found to give excellent resolution for six impurities ► Efficient chromatographic separation was achieved on a C18 stationary phase in simple isocratic mode ► Forced degradation study confirmed the stability indicating nature of the method ► Major oxidative degradant was identified as niacinamideN-oxideDevelopment and Validation of LC/ESI-MS Method for the Detection and Quantification of Exogenous Ceramide NP in Stratum Corneum and Other Layers of the Skin
07 November 2011, 22:04:47
Publication year: 2011
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 6 November 2011
Fitsum F. Sahle, Stefan Lange, Bodo Dobner, Johannes Wohlrab, Reinhard H.H. Neubert
Ceramides (CERs) are integral parts of the intercellular lipid lamellae of the stratum corneum (SC), which provide the barrier function of the skin. Administration of CERs deep into the SC may help to restore the barrier function in affected or aged skin. However, quantification of the amount of CER penetrated into the target site needs a selective and sensitive analytical method. Therefore, an LC/ESI-MS method was developed and validated for the detection and quantification of exogenous CER [NP] in the SC as well as other skin layers. The strategy involved synthesis of ceramide [NP]-D3-18 (deuterated CER [NP]) to distinguish it from the endogenous CER [NP] in MS on weight basis. The method was linear over 10 to 800 ng/ml and sensitive with a limit of detection (LOD) and limit of quantification (LOQ) of 3 and 10 ng/ml, respectively. It was also accurate with within-run and between-run percentage recoveries of 97.1-103.2 and 99.0-104.9, respectively. The within-run and between-run relative standard deviations (RSDs) were 0.9-5.4% and 2.1-7.4%, respectively, suggesting the method is precise. The method was highly selective and the matrix effect was too minimal with matrix factor (MF) mean and RSD values of 1.002 and 4.57%, respectively.
Source: Journal of Pharmaceutical and Biomedical Analysis, Available online 6 November 2011
Fitsum F. Sahle, Stefan Lange, Bodo Dobner, Johannes Wohlrab, Reinhard H.H. Neubert
Ceramides (CERs) are integral parts of the intercellular lipid lamellae of the stratum corneum (SC), which provide the barrier function of the skin. Administration of CERs deep into the SC may help to restore the barrier function in affected or aged skin. However, quantification of the amount of CER penetrated into the target site needs a selective and sensitive analytical method. Therefore, an LC/ESI-MS method was developed and validated for the detection and quantification of exogenous CER [NP] in the SC as well as other skin layers. The strategy involved synthesis of ceramide [NP]-D3-18 (deuterated CER [NP]) to distinguish it from the endogenous CER [NP] in MS on weight basis. The method was linear over 10 to 800 ng/ml and sensitive with a limit of detection (LOD) and limit of quantification (LOQ) of 3 and 10 ng/ml, respectively. It was also accurate with within-run and between-run percentage recoveries of 97.1-103.2 and 99.0-104.9, respectively. The within-run and between-run relative standard deviations (RSDs) were 0.9-5.4% and 2.1-7.4%, respectively, suggesting the method is precise. The method was highly selective and the matrix effect was too minimal with matrix factor (MF) mean and RSD values of 1.002 and 4.57%, respectively.
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