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In this paper, a simple, low cost, highly sensitive voltammetric method for determination of tetrahydropalmatine was described, which was based on a new electrochemical sensor, poly (L-glutamic acid) functionalized electrochemical reduction graphene oxide modified glassy carbon electrode. The electrochemical behavior of tetrahydropalmatine was investigated in detail and some dynamic parameters of electrode process were calculated for the first time. Due to large surface area and good conductivity of proposed sensor, a wider linear range (3.0×10 −7 –2.0×10 −5 mol L −1 ) and lower detection limit (1.0×10 −7 mol L −1 ) were achieved for determination of tetrahydropalmatine. Meanwhile, the proposed method was used in determination of tetrahydropalmatine in Rhizoma Corydalis with well results. [ABSTRACT FROM AUTHOR]

Abstract: The paper presented with qualitative and quantitative analysis of alkaloids in solid-state, using the excitations within the THz-spectroscopic region of 300–30cm−1 (9.00–0.9THz). Series of nine plant flavonoids (FLs) and their mixtures were analyzed both qualitatively and quantitatively. For first time in the literature was reported the quantitative analysis of alkaloids and their mixtures within the THz-region using the solid-state Raman spectroscopy, and matrix-assisted laser desorption/ionization (MALDI) mass spectrometry (MS). The calibration and validation, concentration limit of detection (LOD), limit of quantification (LOQ), and linearity limit (LL) were obtained. The chemometric nonlinear and linear approaches for analysis and interpretation of the quantities were applied. The results obtained were compared with a parallel QA, using the calibrated and validated HPLC electrospray ionization (ESI) mass spectrometric method, electronic absorption (EAs) and CD spectroscopy. The metrology, including accuracy, measurement repeatability (intra-serial precision condition of measurement), measurement precision, trueness of the measurement, and reproducibility of the measurement, measurement bias and errors of the measurements were discussed. [Copyright &y& Elsevier]

Abstract: The quantitative determination of boldine alkaloid in boldo leaf extracts by employing cyclic voltammetry, at a liquid/liquid interface as well as the validation of this methodology against the reference method, high performance liquid chromatography (HPLC), are reported in the present paper. The voltammetric analysis was performed successfully and economically using two kinds of liquid/liquid interfaces: water/1,2-dicholoroethane and water/PVC (polyvinyl chloride)–gelled 1,2-dichloroethane. Linear calibration curves in the concentration range of 1.04×10−5 molL−1 to 5.19×10−4 molL−1 were obtained with a detection limit equal to (6.1±0.7)×10−5 molL−1 and the quantitative determination of this alkaloid, in complex matrixes such as boldo leaf extracts, by the electrochemical technique proposed was found to be equal to the values obtained using the standard HPLC method. The validation analysis of this methodology against HPLC demonstrated that accuracy, linearity, limit of detection (LOD), limit of quantification (LOQ), specificity and precision are acceptable. The electroanalytical technique proposed is economical and selective, involves simple equipment and can be applied for the quantitative determination of boldine alkaloid in complex matrixes such as leaf extracts without special drug separation. Moreover, cyclic voltammetry (CV) experiments applied at the liquid/liquid interface under different experimental conditions allowed us to study the transfer mechanism of boldine, and determine a value of pK a w =6.90 for protonated boldine, from the variation of voltammetric peak current with pH. [ABSTRACT FROM AUTHOR]

Abstract: Ultra-performance liquid chromatography–quadrupole-time-of-flight mass spectrometry (UPLC–Q-TOF-MS) is an effective technique for analysis of complex samples with offering rapid, efficient separation in combination with accurate mass measurement and tandem mass spectrometry (MS/MS). This paper exploits this technique to identify the alkaloids in corydalis yanhusuo, an important antalgic Traditional Chinese Medicine (TCM). The mass spectral fragmentation behavior of one tertiary alkaloid and two quaternary alkaloids was studied in detail. Low-abundance product ions of tertiary and quaternary alkaloids were investigated and compared between each other. Sixteen alkaloids were screened out by using a systematic screening method developed in our laboratory; structures of eight therein were identified by characteristic UV absorption spectrum and positive ion mode of Q-TOF-MS/MS; and two of them were discovered for the first time in corydalis yanhusuo to our knowledge. This research demonstrates the potential of UPLC-Q-TOF-MS in structural characterization and identification of components in traditional Chinese herbal medicines. [Copyright &y& Elsevier]

Abstract: The spectroscopic characterizations of solid substrate room temperature phosphorescence (SS-RTP) of palmatine (Pal) have been studied. Strong RTP signal at 615nm can be induced on filter paper in the presence of TIAc. The interaction between calf thymus DNA (ctDNA) and Pal has been investigated at pH 6.90 using fluorescence, UV–vis, SS-RTP and cyclic voltammogram spectroscopy. Strong binding affinity of Pal with DNA is revealed from the absorption and fluorescence studies in the liquid state. With the addition of ctDNA, the fluorescence intensity of Pal is enhanced greatly and UV–vis spectra show no apparent hypochromicity and red shift, which indicates that Pal intercalates into ctDNA bases. However, this conclusion could not explain the phenomena from fluorescence polarization and denatured DNA measurements, which indicate that groove binding is at least the main binding mode. Binding constant and binding site size have been calculated to be 2.57×104 L/mol and 0.16 based on Scatchard plot from fluorescence titration data. Groove binding has also been supported by phosphorescence lifetime and anion quenching experiments. Above studies demonstrate that there should exist intercalative binding and groove binding in the interaction of Pal and DNA. Furthermore, cyclic voltammogram study suggests that electrostatic binding exists at the same time exactly. Taken together, the binding model obtained in this study is mixed-mode. [Copyright &y& Elsevier]

In this paper, perhydroxyl-cucurbit[6]uril ((HO)12CB[6]) was, for the first time, grafted to silica gel as a hydrophilic-interaction chromatographic stationary phase. Several alkaloids were used as probes to investigate the retention mechanism on the new stationary phase. The effect of mobile phase variables such as acetonitrile content, ionic strength and pH on their chromatographic behavior was investigated. The results indicate that the stationary phase behaves as a hydrophilic-interaction chromatographic packing. Finally, several alkaloids were separated on the stationary phase. [Copyright &y& Elsevier]

A novel, rapid and accurate method for the separation and determination of aloperine (ALP), sophoridine (SRI), matrine (MT) and oxymatrine (OMT) has been developed by combination of flow injection (FI) with microfluidic capillary electrophoresis (CE) for the first time. In the present paper, a continuous sample introduction interface was described. The interface with an H-channel structure was produced using a non-lithographic approach. The H-channel structure was fixed on a planar plastic base utilizing a horizontal 6.5 cm-long separation capillary with two vertical sidearm tubes on each end that served as inlet and outlet flow-through electrode reservoirs. The inlet reservoir also functioned as interface for coupling to the FI system. The buffer solution used was a 50 mmol l−1 borate solution with the pH adjusted to 8.80 with 2 mol l−1 HCl. The performance of the system was demonstrated in the separation and determination of ALP, SRI, MT and OMT with UV detection at 215 nm, achieving baseline separation within 2 min. A series of samples was injected repeatedly without current interruption and subsequent rinsing, and the contents of these four bio-alkaloids in two marketed drugs were determined with satisfactory recovery by this proposed method. [Copyright &y& Elsevier]