固相萃取-反相高效液相色谱法同时测定血清中3种抗癫痫药物

目的应用固相萃取-反相高效液相色谱法测定血清中抗癫痫药物。方法用Elut Bond C18小柱预处理样品，甲醇为洗脱剂；采用Waters Nova RC18柱，流动相为甲醇：水-45：55；检测波长230nm，流速1ml／min，内标(苯乙酮)法定量。结果苯巴比妥、苯妥英、卡马西平的浓度线性范围分别为4．1～62．6μg／ml(r=0．9968)、3．9～60．1μg／ml(r=0．9971)和1．6～21．2μg／ml(r=0．9945)，最低检测限分别为0．05μg／ml、0．05μg／ml和0．01μg／ml；相对回收率分别为90．6％～103．6％、93．4％～118．3％和91．2％～101．1％；批内变异系数均小于6．0％，批间变异系数均小于8．0％。结论固相萃取-反相高效液相色谱法简便、灵敏、准确、稳定，适合于以上3种抗癫痫治疗药物的同时监测。     

固相萃取反相高效液相色谱法测定全血环孢素A

目的　建立固相萃取反相高效液相色谱法测定全血环孢素A的方法。方法　全血中的环孢素A采用Wa tersSep PakC18萃取小柱提取浓缩 ,色谱柱WatersNova PakC18;流动相　乙腈∶甲醇∶水 (32 0∶30∶15 0 ,V/V) ;流速 0 6 5ml/min ;检测波长 2 0 6nm ,环孢素D作内标。结果　方法的回收率为 95 8% ,相对标准差 (RSD)为 7 5 % ,线性范围为5 0～ 2 0 0 0 μg/L ,r=0 9999。 结论　该方法特异、敏感、准确 ,可用于全血环孢素A的测定。     

RP-HPLC测定丹参舒心胶囊中丹参酮ⅡA的含量

目的：建立丹参舒心胶囊中丹参酮ⅡA的含量测定方法。方法：采用反相高效液相色谱法测定含量。色谱柱为Diamonsil C18;流动相为乙腈-甲醇-氯仿-水（42∶40∶1∶18）;流速为1.0 ml/min;检测波长为270 nm。结果：丹参酮A在0.162~2.700μg范围内与峰面积成良好的线性关系（r=1.000 0）;平均加样回收率为99.90%（n=5）,RSD=0.4%（n=5）。结论：本法灵敏、准确,重现性好,可用于丹参舒心胶囊中丹参酮A的含量测定。     

高效液相色谱法测定香砂养胃丸中的橙皮式甙含量

目的　以反相高效液相色谱法测定香砂养胃丸中橙皮甙的含量。方法　色谱柱为Noca PakC18( 3 9mm× 15 0mm) ;流动相 :5 %甲醇 :乙晴 ( 85 :15 ) ,流速 1ml/min ,检测波长 :2 84nm。结果　橙皮甙在 10～ 5 0 μg/ml范围内线性关系良好 (r =0 9999) ,日内、日间差异小于 8%,平均回收率为 10 1 46 %。结论　该方法简便准确 ,适用于对该制剂的控制。     

高效液相色谱法对新型吡啶类活性物质XY-4的纯度测定

目的建立新型吡唑[3,4-b]吡啶类活性物质XY-4的高效液相色谱法测定含量的方法。方法采用高效液相色谱法,以Phenomenex Gemini 5μm C18 110(4.6 mm×250 mm,5μm)为色谱柱,甲醇-水(75∶25)为流动相,流速1 ml/min,柱温30℃;检测波长为230 nm。结果 XY-4的量在20~100μg/ml的浓度范围内与峰面积积分值线性关系良好(r=0.9999),平均加样回收率为97.6%,RSD为1.45%。结论该方法简便易行,准确可靠,可用于指导XY-4的合成。     

高效液相色谱-质谱联用法测定人体内阿奇霉素血药浓度

目的建立高效液相色谱法测定人体内阿奇霉素血药浓度的方法。方法采用高效液相色谱紫外检测-质谱联用法,色谱柱CLC-CN分析柱（250 mm×4.6 mm,5μm）,流动相：0.1 mol/L磷酸二氢钠-甲醇-乙腈（85∶7∶8,pH调节至6.0）,流速1 ml/min,控制柱温为40℃,检测波长为210 nm,定量方法为峰面积外标法。结果阿奇霉素血药浓度线性范围在0.1～4.0μg/ml,r=0.9998,日内精密度1.25%～4.41%,日间精密度2.79%～6.83%。结论高效液相色谱法测定人体内阿奇霉素血药浓度简单快捷、结果准确、灵敏度高、重复性好,值得推广。     

高效液相色谱-荧光检测法快速测定脊髓和脑内氨基酸

目的建立快速测定脊髓和脑内氨基酸浓度的方法。方法通过邻苯二甲醛和β-巯基乙醇柱前衍生、反相高效液相色谱结合荧光(激发波长280nm,发射波长340nm)检测氨基酸浓度。用0.1mol/L磷酸盐缓冲液(pH值6.00~6.25)和甲醇(46%)混合液(加入四氢呋喃2%)作流动相,流速为1ml/min。结果在0.1~40.0μmol/L范围内,氨基酸浓度与相对峰面积之间的相关系数(r)均值为0.9992,日内和日间变异系数(CV)分别为2.41%~5.23%、3.51%~6.48%,平均回收率为90.13%~98.47%。结论本法灵敏度高、快速、简便易行,可用于脊髓和脑内氨基酸测定。     

HPLC测定注射用多西他赛中多西他赛含量

目的:建立测定注射用多西他赛中多西他赛含量的高效液相色谱法。方法:采用反相高效液相色谱法,色谱柱为Hypersil C18(250mm×4·6mmi.d10μm),以乙腈-水(48∶52)为流动相,检测波长233nm,流速1·0mL/min,柱温为30℃。结果:在6·0~60·0mg/L范围内,多西他赛浓度与峰面积的线性关系良好(r=0·9999),高中低3种浓度的加样回收率为98·58%~101·3%,相对标准差为0·4%~0·67%。结论:所建立的方法准确、简便,适用于注射用多西他赛的质量控制。     

高效液相色谱法同时测定小儿咳喘灵颗粒中麻黄碱和伪麻黄碱含量

目的：建立一种高效液相色谱法同时测定小儿咳喘灵颗粒中麻黄碱、伪麻黄碱含量的方法。方法：以菲罗门Synergi Fuion-RP色谱柱（250×4.6mm,5μm）,甲醇-0.02mol/L磷酸二氢钾溶液为流动相,检测波长为210nm,流速为0.8ml/min,柱温为35℃。结果：盐酸麻黄碱和盐酸伪麻黄碱的线性范围分别为0.001281~0.032025mg/ml（r=0.9999）和0.0001327~0.013274mg/ml（r=0.9996）,平均加样回收率分别为94.67%,RSD=1.4%和94.51%,RSD=2.3%。结论：该方法简便、准确、易行,可用于质量测定。     

高效液相色谱法测定消毒乳膏中非法添加的抗真菌药物

目的 建立同时测定消字号乳膏中灰黄霉素、酮康唑、联苯苄唑、克霉唑、硝酸益康唑、硝酸咪康唑、盐酸萘替芬和盐酸特比萘芬等8种抗真菌药物的高效液相色谱法。方法 采用CAPCELL PAK C18(250 mm×4.6 mm×5μm)色谱柱分离,以乙腈-水为流动相,梯度洗脱,220 nm波长检测,外标法定量消毒乳膏中非法添加的抗真菌药物成分。结果 8种抗真菌组分在0.06~20.86μg/mL范围内线性关系良好(相关系数r=0.999 9),检出限和定量限分别为1.95~6.95 mg/kg和5.85~20.86 mg/kg,平均加标回收率为92.92%~104.05%,相对标准偏差为1.25%~3.80%。市售的20批消字号乳膏中8批样品检出硝酸咪康唑,含量为8.8~23.7 mg/g, 1批样品检出酮康唑,含量为9.7 mg/g。结论 高效液相色谱法可同时测定消字号乳膏中非法添加的8种抗真菌药物。     

Quantitative phase spectroscopy

Quantitative phase spectroscopy is presented as a novel method of measuring the wavelength-dependent refractive index of microscopic volumes. Light from a broadband source is filtered to an ~5 nm bandwidth and rapidly tuned across the visible spectrum in 1 nm increments by an acousto-optic tunable filter (AOTF). Quantitative phase images of semitransparent samples are recovered at each wavelength using off-axis interferometry and are processed to recover relative and absolute dispersion measurements. We demonstrate the utility of this approach by (i) spectrally averaging phase images to reduce coherent noise, (ii) measuring absorptive and dispersive features in microspheres, and (iii) quantifying bulk hemoglobin concentrations by absolute refractive index measurements. Considerations of using low coherence illumination and the extension of spectral techniques in quantitative phase measurements are discussed.     

Gonadotropin in follicular phase in women with luteal phase defect.

Serum FSH and LH in women with luteal phase defect were measured. Their serum FSH and LH were lower than those in normal women and higher than those in women with amenorrhea. Administration of clomiphene citrate to the women with luteal phase defect were effective in 2/3 of the cases. These results are consistent with the hypothesis that a relative deficiency of FSH during the follicular phase results in diminished follicular development and subsequent inadequate corpus luteum maintenance.     

Structured illumination quantitative phase microscopy for enhanced resolution amplitude and phase imaging

Structured illumination microscopy (SIM) is an established microscopy technique typically used to image samples at resolutions beyond the diffraction limit. Until now, however, achieving sub-diffraction resolution has predominantly been limited to intensity-based imaging modalities. Here, we introduce an analogue to conventional SIM that allows sub-diffraction resolution, quantitative phase-contrast imaging of optically transparent objects. We demonstrate sub-diffraction resolution amplitude and quantitative-phase imaging of phantom targets and enhanced resolution quantitative-phase imaging of cells. We report a phase accuracy to within 5% and phase noise of 0.06 rad.OCIS codes: (180.0180) Microscopy, (100.6640) Superresolution, (030.0030) Coherence and statistical optics     

Pressure-driven electronic phase transition in the high-pressure phase of nitrogen-rich 1H-tetrazoles

High-energy-density materials (HEDMs) require new design rules collected from experimental and theoretical results and a proposed mechanism. One of the targeted systems is the nitrogen-rich compounds as precursors for possible polymeric nitrogen or its counterpart in a reasonable pressure range. 1H-tetrazole (CH₂N₄) with hydrogen bonds was studied under pressure by both diffraction and spectroscopy techniques. The observed crystal structure phase transition and hydrogen bond-assisted electronic structure anomaly were confirmed by first-principles calculation. The rearrangement of the hydrogen bonds under pressure elucidates the bonding interactions of the nitrogen-rich system in local 3D chemical environments, allowing the discovery and design of a feasible materials system to make new-generation high-energy materials.

Combined high pressure in situ spectra with first-principles calculations, a possible hydrogen-bond assisted phase transition was proposed in tetrazole.     

Acute phase of stroke

Ictus treatment requires an urgent, coordinated, multidisciplinary effort be carried out. Pharmacological treatment of an acute phase of Ictus is another step in an integrated treatment of our patients. The author will concentrate on the specific pharmacological treatment indicated to care for acute Ictus without dealing with the standard support care nor with the treatment of the most usual complications.