咽炎颗粒的喷雾干燥工艺研究

目的确定咽炎颗粒喷雾干燥的最佳工艺。方法采用正交试验法，以含水量和蒙花苷含量为指标，考察进／出口风温、辅料加入量、浸膏相对密度3个因素对其的影响。结果咽炎颗粒喷雾干燥的最佳工艺条件为：进／出风温度160—165℃／80—85℃，辅料加入量40％，浸膏相对密度1．14。结论本试验为咽炎颗粒干燥工艺的改进提供了依据。     

不同干燥方法对地黄与玄参中环烯醚萜苷类成分含量的影响

目的研究不同干燥方法对地黄、玄参中环烯醚萜苷类成分含量的影响。方法地黄、玄参分别经105℃真空干燥及105℃普通干燥两种方法处理后,取真空干燥组及普通干燥组1、3、5、7、9h的地黄、玄参样品采用高效液相色谱法测定地黄中梓醇和玄参中哈巴俄苷含量。结果随着干燥时间的延长,普通干燥组地黄中梓醇和玄参中哈巴俄苷的含量分别降低60%、80%,与真空干燥组比较有显著性差异,真空干燥组待测成分含量没有明显影响。结论真空干燥较普通干燥的处理方法更有益于环烯醚萜苷类中药。     

电离辐射诱导小鼠骨电子顺磁共振信号检测的影响因素

目的 研究影响小鼠骨辐射诱导电子顺磁共振（EPR）信号检测的因素。 方法 将小鼠股骨去除软组织和骨髓,干燥,制成股骨段,经60Co γ射线照射,照射剂量率为5 Gy/min,照射剂量为10 Gy和50 Gy。检测不同干燥程度、检测方向、微波功率和叠加次数等条件下骨EPR的信号强度。 结果 降低骨样品含水量、设置合适的微波功率、增加叠加次数均可以增加样品信号强度,且不同检测方向下同一份样品的信号强度有一定差异。 结论 适当的样品预处理和检测参数设定可以提高骨EPR检测的灵敏度,样品多方向检测并取平均值可减弱骨样品不均一产生的影响。     

用ФОР-ТВЗКС放化分离~(90)Y

直接从溶解的样品中分离~(90)Y的方法是萃取分析法。众所周知,这种分离方法是用Мцомф萃取样品中所含的~(90)Y,并测量其在有机相中的活度。但在此条件下,若测定钇的产额则往往是困难的。现工作是验证从溶解的样品中,析出钇和用ФОР-ТВЗКС分离掉其杂质的可行性。将鳕鱼和黑背鲱鱼的骨骼放在105°～110℃烘干,然后在400～450℃下灰化2小时。取50～75克灰样用浓硝酸浸湿.加入准确量放射性活度的~(90)Sr+~(90)Y。样品在尽最少的浓硝酸中加热溶解,往溶液中加入一定量的锶和钇的稳定性同位素作载体。钇量按下述计算加入:其流入到交换柱中的含量不超过5mg/cm~3 ТВКС。所得的溶液用NH_4OH将酸度调节到0.2mol/l。将100ml体积的试液流经装有     

旋覆花水提物的TLC和HPLC特征图谱及6种化学成分的含量测定

目的 建立旋覆花水提物的薄层色谱(TLC)和高效液相色谱(HPLC)的特征图谱,同时建立水提物中6种成分(绿原酸、咖啡酸、异槲皮苷、1,5‐二咖啡酰奎宁酸、4,5‐二咖啡酰奎宁酸和旋覆花内酯)的含量测定方法,评价11批旋覆花药材水提物的相似性。方法 (1)采用HF₂₅₄型薄层层析硅胶板、正丁醇‐丙酮‐吡啶‐水‐冰醋酸(1∶5∶3∶1∶10μL)为展开剂,在365 nm波长下检视喷洒10%硫酸‐乙醇前、后的色谱斑点,建立TLC特征图谱。(2)采用Sino‐Chrom ODS‐BP(4.6 mm×250 mm,5μm)色谱柱,流动相为0.05%磷酸溶液‐乙腈的梯度洗脱程序,流速0.8 mL/min,柱温35℃,检测波长205 nm,建立HPLC特征图谱。(3)6种成分的含量测定条件与(2)相同,但检测波长分别为203 nm(旋覆花内酯)、256 nm(异槲皮苷)和327 nm(咖啡酸、绿原酸、1,5‐二咖啡酰奎宁酸、4,5‐二咖啡酰奎宁酸)。结果 (1)喷洒显色剂前、后的TLC图谱均显示出良好的特征性。(2)HPLC特征图谱显示含有28个共有峰,指认出10个峰(绿原酸...     

高效液相色谱-荧光检测法测定人血浆中福多司坦含量

目的建立快速测定人血浆中福多司坦药物浓度洗脱的高效液相色谱-荧光检测法。方法采用高效液相色谱反相柱,流动相：20 mmol/L醋酸钠溶液（含0.6%四氢呋喃,pH7.2）-乙腈（81.5∶18.5）,荧光检测,激发波长：338 nm;发射波长：450 nm。样品与邻苯二甲醛经2-巯基乙醇衍生反应,三氯乙酸沉淀蛋白,离心,上清液进样测定。结果福多司坦血浆浓度定量限和检测限分别为0.20、0.05μg/ml,在0.25~80μg/ml范围内,峰面积与浓度呈良好的线性关系（r=0.9995）,RSD为3.5%,平均回收率为96.2%（n=5）。样品贮存稳定性研究表明,冻融（-18℃）下贮存稳定性较室温稳定性高。结论本方法简便、准确,精密度良好,可用于临床福多司坦血浆样品含量的测定。     

芫花根HPLC色谱指纹图谱研究

目的建立芫花根HPLE色谱指纹图谱,为芫花根有效成分筛选、药理毒理学、药物代谢动力学以及脱毒提取工艺研究提供可靠的检测方法。方法利用柱层析(硅胶,Sephadex LH-20)从芫花根乙醇提取物中分离代表性化合物;以HPLE方法,梯度洗脱,分别测定不同地区芫花根各样品10批。色谱条件：流动相A为甲醇;流动相B为水(乙酸调pH为3．0)。梯度洗脱A/B体积比：0～20min,35／65;21～40min,45／55;41～60min,50／50;61～85min,65／35,分析时间120mine,流速：1ml／min,柱温：35℃。结果10批芫花根乙醇提取物得到的色谱指纹图谱有23个共有峰,可分为6个区段。保留时间0～11min出现2小峰;保留时间11～23min出现2个峰;保留时间23～35min出现1峰;35～66min出现14个峰,主要特征峰6,7,11,12,13,18,19号峰在此区域,峰13为最强峰;66～72min出现1个峰,72～85min出现3个峰。不同产地的芫花根指纹图谱有一定差异。结论芫花根乙醇提取物HPLE指纹图谱具有很强的特征性及专属性,可作为检测方法用于芫花根黄酮、香豆素类化合物有效成分筛选、协同作用、药代动力学、毒理学以及芫花根脱毒提取工艺研究。     

HPLC法测定人血浆中克林霉素含量及其药动学研究

目的建立人血浆中克林霉素的HPLC检测方法。方法采用HPLC法检测人血浆中克林霉素含量,检测条件为:色谱柱:InertsilDOS-3 C185μm硅胶柱(250 mm×4.6 mm);流动相:乙腈/0.05 M KH2PO4=30/70(v/v),流速:1 ml/min;柱温:35℃,检测波长:204 nm,进样量为100μl。结果血浆中克林霉素浓度在0.20~16.0μg/ml范围内线性关系良好(r=0.9992~0.9998),最低检测浓度为0.20μg/ml,方法学回收率为82.42%~89.37%,日内及日间精密度RSD<15%。结论此方法专属、准确、灵敏度高,样品处理过程简便,适合克林霉素临床药代动力学研究。     

HPLC法测定盐酸纳洛酮鼻腔喷雾剂的含量及有关物质

目的　建立HPLC法用于盐酸纳洛酮鼻腔喷雾剂的含量及有关物质测定。方法　色谱柱为ApolloODS (15 0× 4 .6 0mm ,5 μm) ;流动相为甲醇 -乙腈 - 0 .0 2mol·L-1的磷酸二氢钾 (1∶1∶8) ;流速 1.0ml/min ;检测波长 2 4 0nm ;外标法峰面积定量。结果　在该色谱条件下 ,中间体、辅料、分解产物等对主药测定无干扰 ;盐酸纳洛酮浓度在 10 .2～ 81.6 μg·ml-1范围内线性关系良好 ,回归方程为Y =110 2 6 .4 1X - 1982 3.96 ,r =0 .9998;最低检出浓度为 5 0ng·ml-1;高、中、低三个浓度日内、日间的RSD在0 .4 9%～ 1.5 1%之间 ;重复性试验RSD为 0 .98% (n =9) ;样品的平均回收率为 99.92 % ,RSD为 0 .70 % (n =9)。结论　该法准确、可靠、重现性好 ,可用于盐酸纳洛酮鼻腔喷雾剂的含量及有关物质的测定     

氨基酸组成分析直接鉴定SDS-PAGE分离的蛋白质

蛋白质组学是后基因组时代研究的重要领域。蛋白质组研究的基本技术包括双向凝胶电泳分离技术、蛋白质鉴定技术、计算机图像数据处理与蛋白质组数据库构建等。氨基酸组成分析［1,2］作为蛋白质组研究中的鉴定方法之一,对质谱鉴定、N端氨基酸序列鉴定等具有补充及验证作用。蛋白质是由20种氨基酸通过肽键连接起来的生物大分子,测定蛋白质的氨基酸组成可获得蛋白质的基本信息。本研究以马心肌红蛋白和细胞色素C为样品,优化实验条件,以此建立一种高灵敏度、高准确度的鉴定双向凝胶电泳分离后的蛋白质点方法。该方法还可用于分析天然蛋白质、基因重组蛋白质。 1 材料和方法 1.1 材料 1.1.1 试剂丙烯酰胺、过硫酸胺、甘氨酸、十二烷基磺酸钠(SDS)、三羟甲基氨基甲烷(Tris)、三氟醋酸(TFA)、无水醋酸钠均为国产分析纯;甲叉双丙烯酰胺为进口分装;乙腈、甲醇为色谱纯;邻苯二甲醛（OPA）溶液、氯甲酸芴甲酯(FMOC)溶液、标准氨基酸溶液、硼酸盐缓冲液（pH 10.2）购自Hewlett Packard公司;邻苯二甲醛、马心肌红蛋白、细胞色素C为Sigma公司产品。 1.1.2 仪器 Hewlett Packard 1100 HPLC自动氨基酸分析仪;转印仪为Bio-Rad 半干转印仪。 1.2 SDS-PAGE电泳 采用15%分离胶,5%浓缩胶;马心肌红蛋白、细胞色素C上样量均为10 μg;聚集电压85 V,1 h;分离电压105 V,3 h;考马斯亮蓝染色。 1.3 电转印 转印缓冲液：0.025 mol/L Tris,0.192 mol/L甘氨酸,20%甲醇;电转印条件：恒电压24 V,1 h。当凝胶上的蛋白质点转印到PVDF膜时,将PVDF膜用水多次漂洗,晾干,待用。 1.4 酸水解 切割PVDF膜上的蛋白质点,放入小玻璃管中,加6 mol/L盐酸400 μl,封口,110℃水解24 h。1.5 氨基酸的提取 将水解后小玻璃管中的样品转移至1 ml样品管中,用氮气吹尽盐酸,并减压抽干。加170 μl提取溶液（水、乙腈和0.1%TFA的比例为50∶100∶20）,充分振摇,超声10 min,除去PVDF膜,冷冻干燥。加40 μl硼酸盐缓冲液,混匀,离心,取上清液,浓缩。 1.6 氨基酸的测定 采用OPA/FMOC柱前衍生方法。色谱条件：色谱柱C18 ODS-Hypersil,5 μm,125 mm×4 mm;柱温40℃;检测波长338 nm,226 nm;流速1 ml/min,进样量1 μl。流动相A：0.02 mol/L醋酸钠,0.018%三乙胺,0.3%四氢呋喃,用10%醋酸调pH至7.2。流动相B：0.1 mol/L醋酸钠（pH 7.2）∶乙腈∶甲醇（20∶40∶40）。洗脱梯度：0.0 min,0%B;17 min,60%B;18.0 min,100%B;24.0 min,100%B;25.0 min,0%B。 1.7 数据库检索 采用Internet上ExPASy蛋白质数据库检索,软件为AACompIdent,选择匹配模型free constellation,按以下各氨基酸之间的摩尔比值输入计算机,Asx,Glx,Ser,Thr,Ala,Pro,Arg,Val,Ilu,Leu,His,Gly,Tyr,Phe。蛋白质酸水解后Cys和Trp几乎被完全破坏,Met,Lys大部分被破坏,因此不输入计算机。Asn和Gln水解后分别为Asp和Glu。     

Knee injury and Osteoarthritis Outcome Score (KOOS) - validation of a Swedish version

The Knee injury and Osteoarthritis Outcome Score (KOOS) is a self-administered instrument measuring outcome after knee injury at impairment, disability, and handicap level in five subscales. Reliability, validity, and responsiveness of a Swedish version was assessed in 142 patients who underwent arthroscopy because of injury to the menisci, anterior cruciate ligament, or cartilage of the knee. The clinimetric properties were found to be good and comparable to the American version of the KOOS. Comparison to the Short Form-36 and the Lysholm knee scoring scale revealed expected correlations and construct validity. Item by item, symptoms and functional limitations were compared between diagnostic groups. High responsiveness was found three months after arthroscopic partial meniscectomy for all subscales but Activities of Daily Living.     

Endovascular management of carotid-cavernous fistulas

Objective To investigate endovascular treatment of traumatic direct carotid-cavernous fistulas （CCF） and their complications such as pseudoaneurysms. Methods： Over a five-year period, 22 patients with traumatic direct CCFs were treated endovascularly in our institution. Thirteen patients were treated once with the result of CCF occluded, 8 twice and 1 three times. Treatment modalities included balloon occlusion of the CCF, sacrifice of the ipsilateral internal carotid artery with detachable balloon, coll embolization of the cavernous sinus and secondary pseudoaneurysms, and covered-stem management of the pseudoaneurysms. Results All the direct CCFs were successfully managed endovascularly. Four patients developed a pseudoaneurysm after the occlusion of the CCF with an incidence of pseudoaneurysm formation of 18.2% （4/22）. A total number of 8 patients experienced permanent occlusion of the ICA with a rate of ICA occlusion reaching 36.4% （8/22）. Followed up through telephone consultation from 6 months to 5 years, all did well with no recurrence of CCF symptoms and signs. Conclusion Traumatic direct CCFs can be successfully managed with endovascular means. The pseudoaneurysms secondary to the occlusion of the CCFs can be occluded with stent-assisted coiling and implantation of covered stents.     

The role of interventional radiology in trauma

Introduction Interventional Radiology has evolved into a specialty having enormous input into the care of the traumatized patient.In all hospitals,regardless of size,the Interventional Radiologist must consider their relationships with the trauma service in order to     

The acutely limping child

Acute limping may be the result of multiple pathologies in children. The differential diagnosis varies based on the age of the child. Irrespective of age, the initial imaging work-up includes AP and frog leg radiographs of the pelvis and ultrasound; MRI may sometimes be helpful. In children less than 3 years, infections and trauma are most frequent. MRI is the imaging modality of choice when osteomyelitis is clinically suspected. Between the ages of 3 and 10 years, transient synovitis of the hip and Legg-Calvé-Perthes disease are main considerations but infection, inflammation and focal bony lesions are also considered. In children over 10 years, slipped capital femoral epiphysis also is considered.     

Diagnóstico ecográfico del neumotórax

The ultrasonographic diagnosis of pneumothorax is based on the analysis of artifacts. It is possible to confirm or rule out pneumothorax by combining the following signs: lung sliding, the A and B lines, and the lung point. One fundamental advantage of lung ultrasonography is its easy access in any critical situation, especially in patients in the intensive care unit. For this reason, chest ultrasonography can be used as an alternative to plain-film X-rays and computed tomography in critical patients and in patients with normal plain films in whom pneumothorax is strongly suspected, as well as to evaluate the extent of the pneumothorax and monitor its evolution.     

Carbohydrate Supplementation during Exercise: Does It Help? How Much is Too Much?

KEY POINTS· Carbohydrate intake during exercise can delay the onset of fatigue and improve performance of prolonged exercise as well as exercise of shorter duration and greater intensity (e.g., continuous exercise lasting about 1h and intermittent high-intensity exercise), but the mechanisms by which performance is improved are different.