高效液相色谱法测定和厚朴酚白蛋白纳米粒中的药物含量

建立高效液相色谱法测定和厚朴酚白蛋白纳米粒中和厚朴酚的含量.采用Lichrospher C118(4.6mm×150mm,5μm)色谱柱,流动相为甲醇-水(80 ∶ 20,V/V),流速为1.0mL/min,检测波长为294nm,柱温为30℃.在此色谱条件下,和厚朴酚的色谱峰面积与质量浓度在0.048-12.5μg/mL范围内线性关系良好(r=0.9999),平均回收率为101.2％,RSD为0.5％.本法准确可靠、简便易行,可用于和厚朴酚白蛋白纳米粒中和厚朴酚的含量测定.     

高效液相色谱法测定千柏鼻炎片中的大黄酚

建立了千柏鼻炎片中大黄酚含量的测定方法.采用Prontosil-C18-ace-Eps (250mm×4.6mm,5μm)色谱柱,流动相为甲醇-水(90∶10,V/V),流速1.0mL·min-1;检测波长为254nm,柱温20℃.大黄酚线性范围为1.3-6.5μg/mL(r=0.9999,n=5),平均回收率为90.01％(RSD=2.0％).结果表明方法简便、准确、重现性好,可用于千柏鼻炎片的质量控制.     

浙产檵木叶中槲皮素和山奈酚的含量测定

建立用反相高效液相色谱法同时测定浙产檵木叶中槲皮素和山奈酚含量的方法.采用Eclipse XDB-C18柱;柱温:25℃;流动相为乙腈-0.4％磷酸水溶液(35 ∶ 65,V/V);流速1.0mL/min;检测波长360nm.结果表明,槲皮素、山奈酚在1-100ng/μL的范围内均具有良好的线性关系(r槲皮素=0.99...     

厚朴酚近红外光谱的2D-COS解析及其在藿香正气口服液模型中应用

以氘代氯仿为溶剂,以中药化学标准品厚朴酚为载体,采用二维相关光谱(Tow-dimensional correlation spectroscopy, 2D-COS)技术,采集近红外光谱(near infrared spectroscopy, NIR),由氘代氯仿纯溶剂与厚朴酚原始光谱的二维相关同步谱可知,厚朴酚在1 365～1 455, 1 600～1 720, 2 000～2 181和2 275～2 465 nm处有特征吸收,其中1 440 nm为酚基O—H伸缩振动基频的一级倍频谱带,1 679 nm为芳基C—H及与芳基相连的甲基C—H伸缩振动一级倍频谱带,2 117, 2 304, 2 339和2 370 nm为芳基C—H伸缩振动、弯曲振动和变形振动的组合频,2 445 nm为芳基相连的甲基C—H弯曲振动基频二级倍频谱带,这些波段为厚朴酚的特征归属。以藿香正气口服液复杂体系为载体,以厚朴酚光谱解析的特征波段与间隔偏最小二乘(interval partial least squares, iPLS)和组合间隔偏最小二乘(synergy interval partial least squares, SiPLS)筛选的特征波段分别建立偏最小二乘(partial least squares, PLS)定量模型,模型的决定系数R2_cal 和R2_pre均大于0.99,校正均方根误差(root mean of square error of calibration, RMSEC),交叉验证均方根误差(root mean of square error of cross validation, RMSECV)和预测均方根误差(root mean of square error of prediction, RMSEP)均较小。结果表明,2D-COS技术解析厚朴酚所得波段建立的定量模型与iPLS和SiPLS波段筛选的模型均相对稳定,这使定量模型的波段选择更具有解释性。该研究为中药化学成分NIR光谱解析特征波段的归属提供方法参考,同时为NIR建模波段筛选提供借鉴和指导。     

原子吸收光谱法测定中药厚朴中的铜、铁和钙

用硝酸-高氯酸（4∶1）混合液对厚朴进行消解,然后采用原子吸收光谱法测定厚朴中铜、铁、钙的含量.结果表明,厚朴中含铜4.41μμg/g,含铁55.5 μg/g,含钙6872.5μg/g,加标回收率在93.6％-100.1％之间.该方法测定中药中金属离子的含量方法简便、快速、灵敏.该结果可为进一步研究厚朴的相关药理作用提供参考依据.     

裂解-气相色谱-质谱联用技术研究厚朴浸膏的热裂解

采用在线热裂解-气相色谱-质谱联用技术(Py-GC-M S),模拟卷烟燃吸状态,对厚朴浸膏的热裂解行为进行研究。结果表明:厚朴浸膏的热裂解产物中共鉴定出49种挥发性成分,含量较高的成分为厚朴酚(27.95%)、4-甲氧基和厚朴酚(21.88%)、和厚朴酚(15.46%)、石竹烯(0.69%)、氧化石竹烯(0.59%)、古巴烯(0.43%)等。厚朴酚、和厚朴酚为厚朴主要活性成分,具有抗氧化、抗抑郁、抗菌等活性。该结果为厚朴浸膏在卷烟中的应用提供理论依据。     

RP-HPLC同时测定白花檵木花中的槲皮素和山奈酚

建立用反相高效液相色谱法同时测定白花檵木花中槲皮素和山奈酚含量的方法。采用Eclipse XDB-C18色谱柱(4.6mm×250mm,5μm);柱温:25℃;流动相为乙腈-0.4%磷酸水溶液(35:65,V/V);流速为1.0mL·min-1;检测波长为360nm。槲皮素在1.08×10-3—1.08×10-1μg·μL-1的范围内具有良好的线性关系(r=0.9999),平均回收率97.23%,RSD为1.26%;山奈酚在1.04×10-3—1.04×10-1μg.μL-1的范围内具有良好的线性关系(r=0.9999),平均回收率99.78%,RSD为0.46%。方法简便、准确、可靠,可作为白花檵木花中槲皮素和山奈酚的定量分析方法。     

顶空固相微萃取气相色谱法快速测定人血中的五氯酚

将全自动顶空固相微萃取装置与气相色谱联用,建立了快速测定人血中五氯酚的新方法.实验优化了人血中五氯酚测定的顶空浓缩和固相微萃取各项技术参数,然后使用毛细管气相色谱法分离,电子捕获检测器定量测定.方法的线性范围为0.05-100μg/L,相关系数r=0.9997,检出限为0.02μg/L;加标回收率为86.7%-92.8...     

咖酚伪麻片中盐酸伪麻黄碱的含量

建立高效液相色谱法测定咖酚伪麻片中盐酸伪麻黄碱含量的方法。色谱柱为C18（150mm×4.6mm×5μm）,流动相为0.05mol/L磷酸二氢钠-甲醇（75∶25）,流速为1mL/min,检测波长为210nm。盐酸伪麻黄碱在0.2155—1.0776μg/g范围内线性良好,r=0.9999;盐酸伪麻黄碱的平均收率为100.92%,RSD值为0.41%（n=5）。此法操作简单,准确性好,可用于咖酚伪麻片中盐酸伪麻黄碱的含量测定。     

反相高效液相色谱法测定尿中α-萘酚、β-萘酚、对硝基酚和间硝基酚

利用反相高效液相色谱法建立了同时检测人尿样中的α-萘酚、β-萘酚、对硝基酚和间硝基酚的新方法。采用DiamonsilTMC18（150mm×4.6mm,5μm）色谱柱分离,以V（甲醇）∶V（乙酸铵缓冲液）=58∶42为流动相,流速为0.75mL/min,柱温为35℃,于波长280nm处检测。当α-萘酚、β-萘酚、对硝基酚和间硝基酚的浓度分别在0.120—19.44、0.106—19.44、0.479—27.80μg/mL和0.439—27.80μg/mL范围内与峰面积呈良好线性关系,RSD分别为3.7%—4.3%、2.4%—3.6%、2.7%—4.9%和2.9%—3.6%（n=5）。本法用于尿中4种物质的同时测定,回收率分别为98.8%、103.8%、97.5%和105.0%,结果满意。     

NIST Handbook of Mathematical Functions,edited by Frank W.J. Olver,Daniel W. Lozier,Ronald F. Boisvert,Charles W. Clark

A comparison is made between the competing processes of x-ray scattering and photoelectric absorption. The latter topic is then developed more fully, particular attention being paid to absorption fine-structure and its relevance to the study of the unoccupied energy levels available to electrons in solids. Electron wave scattering theories of metal fine-structure are outlined, together with the simultaneous plasmon emission concept for transition metals and the bound ejected electron theory for the solid halides of potassium.     

质谱仪的发明者阿斯顿半

英国实验物理学家阿斯顿因发明质谱仪分离同位素而获得1922年诺贝尔化学奖.他只拥有学士学位,这在诺贝尔奖的获得者中是不多见的.他是怎样取得成功的,又为何能取得成功?是值得我们去探究的.文章着重介绍了阿斯顿的研究历程,并分析其成功经验,以为今天所倡导的创新研究提供借鉴.     

Zum Diskussionsbeitrag von W. Brauer

Ohne Zusammenfassung

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Percy W. Bridgman's second century

Percy Williams Bridgman's impact on science began in 1909 with his first three experimental papers. These publications on high pressure calibration, techniques, and compressibility, together with the many articles that followed, established his influence on the course of modern high pressure research. Grounded in classical thermodynamics and practical mechanics, his developments showed how the variable of pressure leads to myriad transformations in materials. Studies carried out under a broader range of conditions now provide unprecedented insights into chemical and physical properties at multimegabar pressures and temperatures from millikelvins to thousands of degrees, where novel electronic, magnetic, and superconducting phases are now being discovered. With careful attention to experimental techniques and material performance, Bridgman extended the available pressure range that could be achieved in the laboratory with the development of new devices. We are now witness to continued refinement of static and dynamic compression methods and in situ measurement techniques, including the marriage of high pressure methods with large facilities such as synchrotron, neutron, and laser sources. Bridgman showed the broad range of implications of this work; the modern field of high pressure research now spans physics and chemistry, geosciences and planetary science, materials science and technology, and biology. Selected examples illustrate Bridgman's impact and legacy in this, his second century. For dense hydrogen, new insights have been obtained from high P–T measurements as well as studies of alloys and compounds of hydrogen, leading to the creation of new metallic and superconducting phases. Studies of other hydrogen-rich systems provide both tests of fundamental theory and potentially useful materials for hydrogen storage. High pressure studies of oxides have led to new ferroelectric and multiferroic materials and phases with remarkable properties that guide the design and fabrication of new devices. With the discovery of super-Earths outside our solar system, the high pressure properties of silicates, oxides, volatiles, and the full complement of planetary materials are now problems of cosmic importance well beyond the conditions found on and within the Earth. Developments in high pressure biology are addressing the question of the depth of the biosphere, the processes and reservoirs of carbon in our planet, and new insights into the origins of life as we know it, as well as the possibility of extraterrestrial life. Improved materials that can withstand high P–T conditions and other extreme environments include new forms of diamond, which are advancing experimental methods and finding numerous applications in advanced technology. These developments dovetail with synergetic advances in a broad spectrum of radiation techniques including coherent X-ray, intense neutron, and ultrabright laser sources.