Novel magnetic solid-phase extraction using carboxylated multiwalled carbon nanotubes was proposed with ultra high-performance liquid chromatography–tandem mass spectrometry for the determination of silodosin in biological samples. The effects of various experimental parameters including adsorbent amount, pH, adsorption time, desorption conditions, and adsorbent reusability were systematically validated. Under the optimized conditions, the calibration curve was linear within the concentration range of 1.0–800 ng mL−1 with the correlation coefficient of 0.9997 and the lower limit of detection was 0.3 ng mL−1. The extraction recoveries were over 90.0% with relative standard deviation (RSD) of less than 5.0%. All these results suggested that magnetic extraction method can be used for enrichment and quantification of silodosin in biological samples.
Authors:Y. Chen, X. Li, F. Chen, Q. Zhu, and J. Luo
A rapid, simple, and practical high-performance liquid chromatographic method (HPLC) was developed and validated for the simultaneous determination of norephedrine (NME), norpseudoephedrine (NMP), ephedrine (E), pseudoephedrine (PE), and methylephedrine (ME) in traditional Chinese medicines (TCM) which contained Ephedrae Herba (Ephedra). This analysis could be accomplished within 12.5 min with an Alltima Phenyl Column by isocratic elution using a mixture of KH2PO4 (20 mM)-acetonitrile (96:4, v/v) as the mobile phase at a flow-rate of 0.6 mL min−1 and a wavelength of 210 nm. This method was successfully applied to quantify ephedra alkaloids in both Ma-xing-gan-shi decoction and Ephedra decoction. The concentration of total ephedra alkaloids (4.62 mg mL−1) in Ma-xing-gan-shi decoction was much lower than that (7.10 mg mL−1) in Ephedra decoction. Furthermore, the concentration of NME, NMP, E, PE, and ME was significantly lower in Ma-xing-gan-shi decoction than that in Ephedra decoction, respectively. The method was easily acceptable and would be popular with most analytical laboratories.
Authors:Q. Zhang, Z. Qian, L. Pan, H. Li, and H. Zhu
Berberine, a primary pharmacological active constitute of Coptidis Rhizoma, could inhibit neuronal apoptosis in cerebral ischemia. Here, we aimed to investigate whether and how HIF-1 is implicated in the anti-apoptosis effect of berberine on neurons under hypoxia/ischemia. Viability of PC12 cells treated with berberine prior to or following CoCl2-induced hypoxia was evaluated. Annexin V-PI staining was employed to analyse cell apoptosis ratio. HIF-1α and apoptosis-associated molecules were detected via Western blotting. TUNEL and immunohistochemistry were used to demonstrate apoptosis, HIF-1α and p53 levels in cerebral tissue of middle cerebral artery occlusion (MCAO) rats. Berberine pretreatment promoted PC12 cells survival and inhibited apoptosis under hypoxia condition. At the same time, it decreased cell viability and enhancement of apoptosis were observed with berberine treatment under hypoxia. Decreased HIF-1α, caspase 9, caspase 3 and increased Bcl-2/Bax ratio were responsible for the anti-apoptosis of berberine pretreatment. However, pro-apoptosis by berberine under hypoxia was indicated with opposing regulation of those molecules. Significant reduction of apoptosis, HIF-1α and p53 were found in cerebral tissue of MCAO rats treated with berberine. The present study suggests that berberine regulates neuronal apoptosis in cerebral ischemia, which might be dependent on the degree of cell injury. HIF-1 and the followed apoptotic pathway are involved in those effects of berberine.
Authors:H. Yang, Hua Yin, Z. Wang, L. Fan, Q. Li, and X. Zhu
Traditional Chinese medicine (TCM) has been widely used in many countries for thousands of years and played an indispensable role in the prevention and treatment of diseases, especially the complicated and chronic ones. However, the application of TCM in diseases is still not fully recognized by people around the world, the main reason is that Chinese herb is a very complex mixture containing hundreds of different components. Thus, it is essential to make quality control and evaluation of TCM. A new quality evaluation method, quantitative analysis of multi-components by single marker (QAMS), was developed to the quality control of alkaloids in TCM, a case study on Radix aconiti lateralis, named Fuzi in Chinese. Six alkaloids, including aconitine, hypaconitine, mesaconitine, benzoylaconine, benzoylmesaconine, and benzoylhypaconine, were selected as main components to evaluate the quality of Radix aconiti lateralis. The feasibility and accuracy of QAMS were checked by the external standard method, and various high-performance liquid chromatographic instruments and chromatographic conditions were investigated to verify its applicability. Using aconitine as the internal reference substance and the content of aconitine was calculated according to relative correction factors by high-performance liquid chromatography. The present results showed that there was no significant difference observed between the QAMS method and the external standard method with the relative average deviations less than 3.0%, and QAMS is an effective way to control the quality of herbal medicines and seems to be a convenient and accurate approach to analyze multi-composition when reference substances are unavailable.
Authors:Q. Chen, P. Li, B. Li, F. Yuan, X. Li, and J. Zhu
A rapid and sensitive method for the identification and quantification of yohimbine in Pausinystalia yohimbe is described. The method used is liquid chromatography-quadrupole ion trap mass spectrometry (LC-QIT/MS). The yohimbine standard solution was directly infused into the ion trap mass spectrometers (IT/MS) for collecting the MSn spectra. The major fragment ions of yohimbine were confirmed by MSn at m/z 355, 224, 212, and 144, in the positive-ion mode. The possible main fragment ion cleavage pathway was studied. Yohimbine provided good signals corresponding to the protonated molecular ion [M + H]+. The method is reliable and reproducible, and the detection limit is 0.1 ng mL-1. The method was validated in the concentration range 0.1–50 μg mL−1; the intra- and interday precision ranged from 1.36% to 2.73% and the accuracy was 96.5–108.2%. The mean recovery of yohimbine was 97.1–101% with a relative standard deviation (RSD) <1.93%. The LC-IT/MS method was successfully applied to determine the yohimbine in P. yohimbe.
The study investigated the effects of environmental factors (salinity, pH, ions and activation media) on sperm motility (activation rate, duration of quick movement, and lifespan) and fertilization rate of Phascolosoma esculenta. The results showed that spermatozoa in the coelom and nephridium are able to move quickly. The optimal salinity was 14.64 to 43.35 and the optimal pH was 6.46 to 9.53 for sperm activation and motility, whereas the ranges for fertilization were narrower (18.56 to 30.3 for salinity and 6.46 to 8.61 for pH). Of the ions studied, Na+ was indispensable for sperm motility and fertilization, and Ca2+ and Mg2+ were necessary for fertilization. P. esculenta sperm could not fertilize eggs and have short lifespans in 200 to 600 mmol/L NaCl and KCl solutions. Furthermore, they could not be activated or move in 200 to 600 mmol/L CaCl2, MgSO4, and sucrose solutions.
Authors:H. W. Zhao, Y. L. Geng, H. Zhu, P. Yang, and J. Q. Yu
Seven compounds, including two flavanones, dihydrokaempferol (1) and naringenin (2), and five terpenoids, boscartol A (3), 3,7-dioxo-tirucalla-8,24-dien-21-oic acid (4), 3α-acetoxyl-7-oxo-tirucalla-8,24-dien-21-oic acid (5), 11-keto-β-boswellic acid (6), and acetyl-11-keto-boswellic acid (7), have been purified by high-speed counter-current chromatography (HSCCC) from olibanum. For the separation, from 250 mg of the crude extract, 3.1 mg of 1 (95.2% purity), 2.7 mg of 2 (96.1% purity), 9.1 mg of 3 (96.7% purity), 4.5 mg of 4 (95.3% purity), 5.4 mg of 5 (96.3% purity), 48.1 mg of 6 (96.8% purity), and 45.5 mg of 7 (98.1% purity) were obtained by HSCCC with petroleum ether–ethyl acetate–methanol–water (1:0.8:1.1:0.6, v/v). The structures of these seven compounds were elucidated by a combination of electrospray ionization mass spectrometry (ESI–MS) and extensive nuclear magnetic resonance (NMR) spectroscopic.
Authors:J. Chen, Q. Chen, F. Yu, H. Huang, P. Li, J. Zhu, and X. He
A rapid and sensitive method for the identification and quantification of phillyrin (POG) in Forsythia suspense is described. The phillyrin standard solution was directly infused into the ion trap mass spectrometers (IT-MS) for collecting the MSn spectra. The electrospray ionization (ESI) mass spectral fragmentation pathway of phillyrin was proposed, and the ESI-MSn fragmentation behavior of phillyrin was deduced in detail. The major product ion at m/z 355 belongs to furofuran, which was formed by loss the glucopyranoside (180 Da), and the characteristic fragment ions m/z 473, 395, 337, 309, and 249 were observed. The loss of 18 Da could arise from two different fragmentation pathways, and the observed ion was composed of a mixture of two different structural ions. Quantification of phillyrin was assigned in positive-ion mode at a product ion at m/z 557 → 355 by liquid chromatography-mass spectrometry (LC-MS). The LC-MS method was validated for linearity, sensitivity, accuracy, and precision and then used to determine the content of the phillyrin. Lastly, the LC-MS method was successfully applied to determine phillyrin in real sample F. suspense and three of its medicinal preparations in the positive mode at the first time.
Authors:C. Li, C. Wang, X. Liu, Z. Zheng, L. Wang, Q. Zhu, M. Kang, T. Chen, and C. Liu
In terms of pre-safety assessment of a potential site for high-level radioactive wastes disposal in China, the geochemical
behavior of key radionuclides which tend to be released from the repository must be thoroughly investigated. 99Tc is a long-lived fission product with appreciable productivity in nuclear fuel, and Tc (+7) has unlimited solubility in
near-field geochemical environments. In this study, the effects of ionic strength and humic acid on 99TcO4− sorption and diffusion in Beishan granite were investigated with through-diffusion and batch sorption experiments. Results
indicated that the effective diffusion coefficients (De) of 99TcO4− in Beishan granite varied from 1.07 × 10−12 to 1.28 × 10−12 m2/s without change with ionic strength, while the distribution coefficients (Kd) negatively correlated with ionic strength of the rock/water system. This study also indicates that there is no evident influence
of humic acid concentration on the diffusion behavior of 99TcO4− in Beishan granite, due to the limited interaction between humic acid and 99TcO4−.