UPLC法同时测定阿托伐他汀钙中15个杂质含量

目的建立超高效液相色谱法(UPLC)同时测定阿托伐他汀钙原料药中15个杂质含量的方法。方法采用岛津Shim-pack Velox PFPP(2.1 mm×100 mm,1.8μm)色谱柱,以3.9 g/L醋酸铵缓冲液(pH 5.0):乙腈:甲醇:四氢呋喃(无稳定剂)=67:21:6:6为流动相A,3.9 g/L醋酸铵缓冲液(pH 5.0):乙腈:甲醇:四氢呋喃(无稳定剂)=27:61:6:6为流动相B;梯度洗脱,流速0.43 ml/min,检测波长244 nm,柱温35℃,样品室温度10℃;进样量1.8μl。结果阿托伐他汀钙及各杂质峰间分离良好,在0.3~3μg/ml范围内15个杂质均呈良好的线性关系(r均>0.999,n=6),各杂质平均回收率分别为96.3%,99.1%,99.9%,102.4%,96.4%,99.8%,99.4%,104.9%,106.4%,105.4%,100.1%,98.9%,94.7%,94.4%,101.4%,且不同浓度间平行性良好。15个杂质重复性、进样精密度、中间精密度均良好,48 h内均较稳定。此法除对色谱柱要求较高外,耐用性良好。结论本方法简便、快速、分离度好、专属性强,经方法学验证可用于阿托伐他汀钙原料药杂质质量控制。     

Quantitative UPLC‐MS/MS analysis of chlorogenic acid derivatives in antioxidant fractionates from dandelion (Taraxacum officinale) root

While qualitative studies have identified chlorogenic acids in antioxidant extracts, particularly ethyl acetate‐derived extracts, of Taraxacum officinale, quantitative analysis of these phenolic compounds remains largely unreported for this species. In this study, bioactivity‐guided fractionation of an antioxidant crude ethyl acetate extract (DPPH = 295.481 ± 0.955 mg TE g^?1 extract) from T. officinale root resulted in a number of reverse‐phase fractions that demonstrated high antioxidant activity (DPPH = 1058.733–1312.136 mg TE g^?1 extract), stronger than that of the synthetic antioxidant Trolox^®. UPLC‐MS/MS screening of these fractions for the presence of selected mono‐ and di‐caffeoylquinic acids revealed large quantities of 1,5‐dicaffeoylquinic acid present in several fractions (853.052–907.324 μg mg^?1), respectively. Due to the antioxidant potency and high levels of 1,5‐dicaffeoylquinic acid observed in these fractions, it was concluded that specifically this chlorogenic acid derivative is a major contributor to the antioxidant efficacy of dandelion root.     

S7-200在光纤成缆机上的应用

文中主要介绍用西门子S7-200PLC在光纤成缆机上成功地完成了对西门子S5-135UPLC的改造,最大限度地利用了S7-200的模板扩展功能,极大地节约了改造成本,达到了理想的控制效果.给出了控制方案和软、硬件设计框图,对于相关改造具有较高的应用和参考价值.     

Banana peel: an effective biosorbent for aflatoxins

This work reports the application of banana peel as a novel bioadsorbent for in vitro removal of five mycotoxins (aflatoxins (AFB1, AFB2, AFG1, AFG2) and ochratoxin A). The effect of operational parameters including initial pH, adsorbent dose, contact time and temperature were studied in batch adsorption experiments. Scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR) and point of zero charge (pH_pzc) analysis were used to characterise the adsorbent material. Aflatoxins’ adsorption equilibrium was achieved in 15 min, with highest adsorption at alkaline pH (6–8), while ochratoxin has not shown any significant adsorption due to surface charge repulsion. The experimental equilibrium data were tested by Langmuir, Freundlich and Hill isotherms. The Langmuir isotherm was found to be the best fitted model for aflatoxins, and the maximum monolayer coverage (Q₀) was determined to be 8.4, 9.5, 0.4 and 1.1 ng mg^?1 for AFB1, AFB2, AFG1 and AFG2 respectively. Thermodynamic parameters including changes in free energy (ΔG), enthalpy (ΔH) and entropy (ΔS) were determined for the four aflatoxins. Free energy change and enthalpy change demonstrated that the adsorption process was exothermic and spontaneous. Adsorption and desorption study at different pH further demonstrated that the sorption of toxins was strong enough to sustain pH changes that would be experienced in the gastrointestinal tract. This study suggests that biosorption of aflatoxins by dried banana peel may be an effective low-cost decontamination method for incorporation in animal feed diets.     

Isolation and identification of two major acylated anthocyanins from purple sweet potato (Ipomoea batatas L. cultivar Eshu No. 8) by UPLC‐QTOF‐MS/MS and NMR

In recent years, researches on the isolation and preparation of monomeric anthocyanins have intensified because of the requirements of quantitative and structure–bioactivity relationship analyses. However, simple and effective methods about the scale of monomeric anthocyanins from the natural purple sweet potato powder are rarely reported. In this study, high molecular weight acylated monomeric anthocyanins were isolated from purple sweet potato (Ipomoea batatas L. cultivar Eshu No. 8) via the combination of column chromatography and semi‐preparative HPLC technology and identified mainly by ultra‐high‐performance liquid chromatography quadrupole time‐of‐flight tandem mass spectrometry/mass spectrometry (UPLC‐QTOF‐MS/MS) and ¹H and ¹³C nuclear magnetic resonance (NMR). Two major acylated anthocyanins were unambiguously determined as peonidin 3‐O‐(6‐O‐(E)‐caffeoyl‐(2‐O‐(6‐O‐p‐hydroxybenzoyl)‐β‐D‐glucopyranosyl)‐β‐D‐glucopyranoside)‐5‐O‐(β‐D‐glucopyranoside) and peonidin 3‐O‐(6‐O‐(E)‐caffeoyl‐(2‐O‐(6‐O‐(E)‐feruloyl)‐β‐D‐ glucopyranosyl)‐β‐D‐glucopyranoside)‐5‐O‐(β‐D‐glucopyranoside). The results of this study may help promote the purification of high molecular weight acylated anthocyanins from purple sweet potato as well as from other plant materials in nature.     

Solid lipid nanoparticles of anticancer drug andrographolide: formulation,in vitro and in vivo studies

Diterpenoidal anti-cancer drug andrographolide (AD) was encapsulated into solid lipid nanoparticle (SLN) because of poor aqueous solubility and high lipophilicity. AD-SLNs were prepared by solvent injection method and characterized for droplet size, surface morphology, zeta potential, etc. In vitro drug release was carried out by dialysis-membrane method. A pharmacokinetic study was performed by UPLC/Q-TOF-MS method to determine the maximum plasma concentration (C_max), area under the curve (AUC), etc. There was an improvement in C_max and AUC of AD-SLNs when compared with AD, thereby enhancing the bioavailability of AD. The t_max was increased than that of AD suspension, indicating the sustained release pattern of AD-SLNs. The antitumor activity was carried out on Balb/c mice showing better results with AD-SLNs as compared to AD. Thus, the AD-loaded SLNs would be useful for delivering poorly water-soluble AD with enhanced bioavailability and improved antitumor activity.     

Mass spectrometry of peptides and proteins from human blood

It is difficult to convey the accelerating rate and growing importance of mass spectrometry applications to human blood proteins and peptides. Mass spectrometry can rapidly detect and identify the ionizable peptides from the proteins in a simple mixture and reveal many of their post‐translational modifications. However, blood is a complex mixture that may contain many proteins first expressed in cells and tissues. The complete analysis of blood proteins is a daunting task that will rely on a wide range of disciplines from physics, chemistry, biochemistry, genetics, electromagnetic instrumentation, mathematics and computation. Therefore the comprehensive discovery and analysis of blood proteins will rank among the great technical challenges and require the cumulative sum of many of mankind's scientific achievements together. A variety of methods have been used to fractionate, analyze and identify proteins from blood, each yielding a small piece of the whole and throwing the great size of the task into sharp relief. The approaches attempted to date clearly indicate that enumerating the proteins and peptides of blood can be accomplished. There is no doubt that the mass spectrometry of blood will be crucial to the discovery and analysis of proteins, enzyme activities, and post‐translational processes that underlay the mechanisms of disease. At present both discovery and quantification of proteins from blood are commonly reaching sensitivities of ～1 ng/mL. © 2010 Wiley Periodicals, Inc., Mass Spec Rev 30:685–732, 2011     

Dendrimer as nanocarrier for drug delivery

Dendrimers are novel three dimensional, hyperbranched globular nanopolymeric architectures. Attractive features like nanoscopic size, narrow polydispersity index, excellent control over molecular structure, availability of multiple functional groups at the periphery and cavities in the interior distinguish them amongst the available polymers. Applications of dendrimers in a large variety of fields have been explored. Drug delivery scientists are especially enthusiastic about possible utility of dendrimers as drug delivery tool. Terminal functionalities provide a platform for conjugation of the drug and targeting moieties. In addition, these peripheral functional groups can be employed to tailor-make the properties of dendrimers, enhancing their versatility. The present review highlights the contribution of dendrimers in the field of nanotechnology with intent to aid the researchers in exploring dendrimers in the field of drug delivery.     

Study of hydroxycinnamic acids and malvidin 3-monoglucoside derivatives using capillary zone electrophoresis and ultra-performance liquid chromatography

Model solutions (pH = 3.5, 12% ethanol) of malvidin 3-O-glucoside (Mv3glc), the most common free anthocyanin in grapes and red wines from Vitis vinifera, and three free hydroxycinnamic acids present in wines (caffeic, ferulic and p-coumaric acids) were studied.