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971.
建立了食品中邻苯二甲酸二丁酯(DBP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸二已酯(DEHP)、邻苯二甲酸二正苄酯(DNOP)、邻苯二甲酸二异壬酯(DINP)、邻苯二甲酸二异癸酯(DIDP)6种邻苯二甲酸酯的高效液相色谱-串联质谱检测方法。试样用正己烷∶甲基叔丁基醚∶乙腈(体积比为50∶45∶5)提取并冷冻离心去除脂肪,收集溶剂层并挥干,加入0.5g乙二胺-N-丙基硅烷(PSA)并用2mL乙腈溶液混匀,冷冻离心后过膜备用。优化分离与检测的最佳条件,采用电喷雾正离子电离(ESI+)模式和多离子反应监控(MRM)模式,外标法进行定量。该方法中DBP、BBP、DEHP、DNOP在0.1~3.0mg/L之间,DINP和DIDP在1.0~30.0mg/L之间的线性相关系数R2>0.995;检测限分别为:DBP 0.02mg/L,BBP、DEHP和DNOP 0.005mg/L,DINP和DIDP 0.10mg/L。在添加水平为0.2、0.5、1.0mg/kg时的平均加标回收率和相对标准偏差范围符合食品检测要求。该方法简便、灵敏、精确,适用于检测食品中6种邻苯二甲酸酯残留。 相似文献
972.
设计并合成了二苯磷酰基取代的四苯基硅基团,并将其作为宽禁带聚合物母体材料构筑基元,通过Suzuki反应偶连3,6位取代的咔唑合成了聚合物SiCzP.对聚合物的结构进行了系统的表征.与模型聚合物SiCz相比,二苯磷酰基的强吸电子能力,降低聚合物母体材料的LUMO能级,更有利于电子的注入.SiCzP与SiCz的玻璃化转变温度分别为219与227℃,失重5%时的分解温度分别为441与426℃.二者均具有良好的成膜性,掺杂器件初步结果表明,二苯磷酰基的引入使器件的亮度和效率都得到提高,其最大流明效率和功率效率比SiCz分别提高了98%和75%. 相似文献
973.
974.
以间苯三酚为起始原料,L-脯氨酸为催化剂,经由两步反应首次合成了Empetrifranzinans A(1a,总收率60%)和Empetrifranzinans C(总收率55%),其结构经1H NMR,13C NMR和HR-MS确证。初步药理筛选实验结果表明,1a对人结肠癌、肝癌、胃癌、肺腺癌、卵巢癌细胞表现出了较强的细胞毒作用,其IC50分别为<0.1,1.31,4.90,8.98和3.65μmol·L-1。 相似文献
975.
Yun-Yun Tang Hou-Yu Wang Lu Chen Si Li Chen-Gang Guo Hui-Zhi Fan Cheng-Xi Cao Liu-Yin Fan 《Analytical and bioanalytical chemistry》2013,405(26):8587-8595
We developed a novel polyacrylamide gel electrophoresis (PAGE) method to stack and separate human hemoglobins (Hbs) based on the concept of moving reaction boundary (MRB). This differs from the classic isotachophoresis (ITP)-based stacking PAGE in the aspect of buffer composition, including the electrode buffer (pH 8.62 Tris–Gly), sample buffer (pH 6.78 Tris–Gly), and separation buffer (pH 8.52 Tris–Gly). In the MRB-PAGE system, a transient MRB was formed between alkaline electrode buffer and acidic sample buffer, being designed to move toward the anode. Hbs carried partial positive charges in the sample buffer due to its pH below pI values of Hbs, resulting in electromigrating to the cathode. Hbs would carry negative charges quickly when migrated into the alkaline electrode buffer and be transported to the anode until meeting the sample buffer again. Thus, Hbs were stacked within a MRB until the transient MRB reached the separation buffer and then separated by zone electrophoresis with molecular sieve effect of the gel. The experimental results demonstrated that there were three clear and sharp protein zones of Hbs (HbA1c, HbA0, and HbA2) in MRB-PAGE, in contrast to only one protein zone (HbA0) in ITP-PAGE for large-volume loading (≥15 μl), indicating high stacking efficiency, separation resolution, and good sensitivity of MRB-PAGE. In addition, MRB-PAGE was performed in a conventional slab PAGE device, requiring no special device. Thus, it could be widely used in separation and analysis of diluted protein in a standard laboratory. Figure
Diagram of MRB-induced stacking in a slab PAGE. (A) arrangement of separation buffer (pH 8.01–9.55 Tris–Gly), sample buffer (pH 6.37–7.22 Tris–Gly), and electrode buffer (pH 8.21–9.05 Tris–Gly); (B) initial MRB formed between electrode and sample buffers for stacking of low-content Hbs in sample buffer under electric field; (C) MRB moving toward the anode and partly stacking of Hbs within the MRB; (D) quasi-complete stacking of Hbs via MRB closing to the separating gel; (E) separation of Hbs in a zone electrophoresis mode 相似文献
976.
Yue-Wei Zhang Hai-Yu Yan Ping Fu Fei Jiang Yao Zhang Wen-Xue Wu Jin-Xiang Li 《Analytical and bioanalytical chemistry》2013,405(16):5549-5555
The recognition of targets such as biomacromolecules, viruses and cells by their aptamers is crucial in aptamer-based biosensor platforms and research into protein function. However, it is difficult to evaluate the binding constant of aptamers and their targets that are hard to purify and quantify, especially when the targets are undefined. Therefore, we aimed to develop a modified capillary electrophoresis based method to determine the dissociation constant of aptamers whose targets are hard to quantify. A protein target, human thrombin, and one of its aptamers were used to validate our modified method. We demonstrated that the result calculated by our method, only depending on the aptamer’s concentrations, was consistent with the classical method, which depended on the concentrations of both the aptamers and the targets. Furthermore, a series of DNA aptamers binding with avian influenza virus H9N2 were confirmed by a four-round selection of capillary electrophoresis–systematic evolution of ligands by exponential enrichment, and we identified the binding constant of these aptamers by directly using the whole virus as the target with the modified method. In conclusion, our modified method was validated to study the interaction between the aptamer and its target, and it may also advance the evaluation of other receptor–ligand interactions. 相似文献
977.
978.
979.
Fuqiang Wang Zhonghua Shi Fan Hu Zhengrong Xia Ling Wang 《Analytical and bioanalytical chemistry》2013,405(5):1683-1693
Extraction of phosphopeptides from rather complex biological samples has been a tough issue for deep and comprehensive investigation into phosphoproteomes. In this paper, we present a series of Ti-doped mesoporous silica (Ti-MPS) materials with tunable composition and controllable morphology for highly efficient enrichment of phosphopeptides. By altering the molar ratio of silicon to titanium (Si/Ti) in the precursor, the external morphology, Ti content, internal long-rang order, and surface area of Ti-MPS were all modulated accordingly with certain regularity. Tryptic digests of standard phosphoprotein α- and β-casein were employed to assess the phosphopeptide enrichment capability of Ti-MPS series. At the Si/Ti molar ratio of 8:1, the optimum enrichment performance with admirable sensitivity and capacity was achieved. The detection limit for β-casein could reach 10 fmol, and 15 phosphopeptides from the digest of α-casein were resolved in the spectrum after enrichment, both superior to the behavior of commercial TiO2 materials. More significantly, for the digest of human placenta mitochondria, 396 phosphopeptides and 298 phosphoproteins were definitely detected and identified after enrichment with optimized Ti-MPS material, demonstrating its remarkable applicability for untouched phosphoproteomes. In addition, this research also opened up a universal pathway to construct a composition-tunable functional material in pursuit of the maximum performance in applications. Figure
From human placenta mitochondria to MS 相似文献
980.
Na Guo Dawei Yang Keyume Ablajan Xiaohong Niu Bin Fan Zhiguo Wang Jingang Dai Xiaoxia Wu Baidong Liu 《Journal of separation science》2013,36(12):1953-1958
A rapid analytical method based on rapid resolution LC coupled with MS/MS was first established to quantify seven alkaloids in processed Fuzi decoction. The chromatographic method was optimized to allow simultaneous analysis of all analytes in 5 min and demonstrated good linearity (r > 0.9995), repeatability (RSD < 4.36%), intra‐ and interday precisions (RSD < 5.07%) with good accuracies (97.76–105.08%) and good recovery (95.0–107.5%) of seven alkaloids, namely higenamine, benzoylhypaconine, benzoylmesaconine, benzoylaconine, aconitine, hypaconitine, and mesaconitine. The LODs for these markers were in the range of 2.30–17.00 pg/mL. Quantitative analysis of the seven alkaloids in Baifupian decoction and Heishunpian decoction showed that the content of the seven marker chemicals varied significantly and concluded that the quality of Fuzi was greatly affected by different processed methods. The developed method could be used as a rapid, sensitive, and reliable approach for assessment of the quality of processed Fuzi and related decoction. 相似文献