HPLC法测定不同产地黄蜀葵花中金丝桃苷异槲皮苷及槲皮素-3''''-葡萄糖苷含量

目的测定不同产地黄蜀葵花药材中金丝桃苷,异槲皮苷,槲皮素-3'-葡萄糖苷含量。方法高效液相色谱法。色谱柱:Diamonsil C18柱(150mm×4.6mm,5μm);流动相:乙腈-甲醇(10∶1)-0.4%磷酸,梯度洗脱;检测波长:360nm;柱温:室温;流速:1.0ml/min。结果江苏江堰黄蜀葵花中金丝桃苷含量1.12%,RSD为1.54%;异槲皮苷含量0.68%,RSD为1.58%;槲皮素-3'-葡萄糖苷含量0.59%,RSD为1.47%;江苏兴化黄蜀葵花中金丝桃苷含量0.98%,RSD为1.49%;异槲皮苷含量0.60%,RSD为1.62%;槲皮素-3'-葡萄糖苷含量0.52%,RSD为1.55%;河北邢台黄蜀葵花中金丝桃苷含量1.03%,RSD为1.72%;异槲皮苷含量0.62%,RSD为1.84%;槲皮素-3'-葡萄糖苷含量0.54%,RSD为1.62%。结论江苏江堰黄蜀葵花中金丝桃苷,异槲皮苷,槲皮素-3'-葡萄糖苷含量均最高,江苏兴化黄蜀葵花中金丝桃苷,异槲皮苷,槲皮素-3'-葡萄糖苷含量均最低,该方法简便,准确,重现性好,为各地黄蜀葵花药材的进一步开发利用提供质量控制依据。     

HPLC法测定不同产地黄蜀葵花中金丝桃苷异槲皮苷及槲皮素-3＇-葡萄糖苷含量

目的测定不同产地黄蜀葵花药材中金丝桃苷,异槲皮苷,槲皮素-3＇-葡萄糖苷含量.方法高效液相色谱法.色谱柱：Diamonsil C18柱（150mm&;#215;4.6mm,5μm）;流动相：乙腈-甲醇（10∶1）-0.4%磷酸,梯度洗脱;检测波长：360nm;柱温：室温;流速：1.0ml/min.结果江苏江堰黄蜀葵花中金丝桃苷含量1.12%,RSD为1.54%;异槲皮苷含量0.68%,RSD为1.58%;槲皮素-3＇-葡萄糖苷含量0.59%,RSD为1.47%;江苏兴化黄蜀葵花中金丝桃苷含量0.98%,RSD为1.49%;异槲皮苷含量0.60%,RSD为1.62%;槲皮素-3＇-葡萄糖苷含量0.52%,RSD为1.55%;河北邢台黄蜀葵花中金丝桃苷含量1.03%,RSD为1.72%;异槲皮苷含量0.62%,RSD为1.84%;槲皮素-3＇-葡萄糖苷含量0.54%,RSD为1.62%.结论江苏江堰黄蜀葵花中金丝桃苷,异槲皮苷,槲皮素-3＇-葡萄糖苷含量均最高,江苏兴化黄蜀葵花中金丝桃苷,异槲皮苷,槲皮素-3＇-葡萄糖苷含量均最低,该方法简便,准确,重现性好,为各地黄蜀葵花药材的进一步开发利用提供质量控制依据.     

高效液相色谱法测定水芹中金丝桃苷的含量

目的测定水芹中金丝桃苷的含量。方法采用高效液相色谱法,色谱柱为DiamonsilC18柱(150mm×4.6mm,5μm);乙腈甲醇(10∶1)0.4%磷酸梯度洗脱为流动相;检测波长360nm;流速1.0ml/min。结果金丝桃苷在0.0419～0.2094μg范围内呈良好线性关系,r=0.9993。平均回收率为99.2%,RSD为1.35%。结论本法简便、准确、重现性好,为水芹药材和提取物提供质量控制依据。     

红景天苷衍生物的合成及其抗氧化作用研究

目的设计、合成具有抗氧化、清除自由基作用的新型红景天苷衍生物。方法以红景天苷元-酪醇为先导结构,经结构修饰引入查尔酮结构单元,增强其抗氧化、清除自由基作用。采用DPPH和FRAP法测定其体外抗氧化、清除自由基作用。结果采用微波合成反应,经邻位乙酰化、Claisen-Schmidt缩合以及水解3步反应,制备了一系列含查尔酮结构单元的新型红景天苷衍生物,所有化合物体外抗氧化、清除自由基活性均强于酪醇。结论设计、合成并筛选得到一类新型红景天苷衍生物,构效关系研究证实酚羟基和查尔酮结构单元是化合物抗氧化、清除自由基的重要结构特征。     

高效毛细管电泳法测定白芍总苷胶囊中芍药苷的含量

目的　建立白芍总苷胶囊中芍药苷高效毛细管电泳的含量测定方法。方法　测定条件 ,运行缓冲液 5 0mmol·L-1硼砂缓冲液 (pH 10 .6 ) ;操作电压 2 0kV ;检测波长 2 30nm。结果　测定芍药苷的线性范围为 0 .0 6 2 5～ 1.0mg·ml-1,r =0 .9995 ;白芍总苷胶囊加样回收率为 99.0 7%。日内和日间精密度分别为 1.6 1%和 3.15 %。测定的白芍总苷胶囊中 ,芍药苷的含量结果与HPLC一致。结论　该分析方法简便、快速、准确     

O~6-（对-羧基苄基）鸟嘌呤的合成方法

目的合成作为肿瘤增敏剂和荧光探针分子连结子的新化合物O6-（对-羧基苄基）鸟嘌呤。方法以2-氨基-6-氯嘌呤（ACP）为起始原料,与三乙烯二胺（DABCO）反应生成DABCO-嘌呤,再进行亲核取代反应得到O6-（对-氰基苄基）鸟嘌呤这一重要中间体,最后将氰基水解为羧酸制得O6-（对-羧基苄基）鸟嘌呤。结果与结论合成获得了新结构化合物O6-（对-羧基苄基）鸟嘌呤,其结构经1H-NMR、LC-MS、13C-NMR谱得到确证,总收率为61.4%。重要中间体O6-（对-氰基苄基）鸟嘌呤的制备工艺得到优化,新工艺原料经济易得、操作简单,原子经济效率高、杂质少且易于纯化,适合工业化大生产。     

HPLC法测定银花清咽含片中绿原酸木犀草苷连翘苷含量

目的建立HPLC法测定银花清咽含片中绿原酸、木犀草苷和连翘苷含量的方法。方法 Venusil MP C18柱(4.6 mm×250 mm,5μm),乙腈-0.4%磷酸(10∶90)为流动相,流速:1 ml.min-1,检测波长327 nm,柱温:25℃,检测绿原酸;采用Agilent ZORBAX SB-phenyl柱(4.6 mm×250 mm,5μm),乙腈为流动相A,0.5%冰醋酸为流动相B梯度洗脱,梯度程序为0min(A:10%,B:90%)→15 min(A:18%,B:82%)→30 min(A:18%,B:82%)→40 min(A:30%,B:70%)→45 min(A:40%,B:60%),流速:1 ml.min-1,检测波长:350 nm,柱温:30℃,检测木犀草苷;采用乙腈-水(24∶76)为流动相,流速:1 ml.min-1,检测波长:277 nm,柱温:30℃,检测连翘苷。结果绿原酸、木犀草苷、连翘苷分别在0.3～2.4、0.012～0.096、0.26～2.08μg范围内线性关系良好,平均回收率分别为99.78%、99.90%、100.09%,RSD分别为0.54%、0.46%、0.21%(n=6)。结论该方法重复性好、准确、专属性强,可用于银花清咽片中绿原酸、木犀草苷、连翘苷的含量测定,为较全面地控制银花清咽片的质量提供简便可靠的方法。     

法可林的合成研究

目的 优化白内障药物法可林1的合成工艺,以用于工业化生产.方法 以O-苯二胺为起始原料,经缩合反应、磺化反应制得目标产物法可林1.结果 对反应物配比、催化剂选择、反应温度及时间等因素进行了优化研究,使得该合成反应条件温和,后处理简单,总收率达40.7%,文献收率为24.8%.结论 结构经1H-NMR、MS确证,优化后的工艺更适合工业化生产.     

HPLC法测定红花益气养血胶囊中西红花苷-Ⅰ和西红花苷-Ⅱ的含量

目的建立HPLC法测定红花益气养血胶囊中西红花苷-Ⅰ和西红花苷-Ⅱ的含量。方法色谱柱：Hypersil ODS2C18柱（150 mm×4.6 mm,5μm）,流动相：甲醇-水（48∶52）,检测波长：440 nm;流速：1.0 ml·min-1;柱温：室温。结果西红花苷-Ⅰ在12~45μg·ml-1的浓度范围内线性关系良好（r=1.0000）,平均回收率为99.44%,RSD为1.19%（n=6）;西红花苷-Ⅱ在6.4~24μg·ml-1的浓度范围内线性关系良好（r=0.9999）,平均回收率为98.79%,RSD为1.38%（n=6）。结论本法简便、快速、准确,可用于红花益气养血胶囊中西红花苷-Ⅰ和西红花苷-Ⅱ的含量测定。     

HPLC法同时测定双黄连口服液中绿原酸连翘苷和黄芩苷的含量

目的建立高效液相色谱法测定双黄连口服液中绿原酸,连翘苷和黄芩苷的含量。方法采用Agilent C18分析色谱柱（4.6mm×250mm ID,5μm）;流动相A为5%甲醇（含0.5%磷酸）,流动相B为甲醇;流速：1.0mL/min;洗脱程序：0～35min,A为95%～35%,B为5%～65%;检测波长程序：0～16min为324nm;16～35min为278nm。结果绿原酸、连翘苷和黄芩苷保留时间分别为11.3、26.6、28.0min,与各自相邻峰的分离度〉1.5。以峰面积对进样浓度（μg.mL-1）线性回归,绿原酸、连翘苷、黄芩苷的回归方程分别为：Y=0.035 49X＋0.058 00,r=0.999 9,Y=0.177 0X-0.025 44,r=0.999 9,Y=0.030 69X-0.798 1,r=0.999 9,线性范围分别为14.08～56.32μg.mL^-1,14.34～57.34μg.mL^-1,61.32～245.3μg.m^L-1。绿原酸、连翘苷和黄芩苷回收率分别为99.7%、98.3%和97.8%,RSD分别为0.33%、1.9%和0.55%。结论本方法测定结果与2005年版《中国药典》（一部）测定结果一致,且操作简便,可用于双黄连口服液中绿原酸、连翘苷和黄芩苷含量的同时测定。     

金丝桃苷对正常小鼠免疫功能的影响

目的研究金丝桃苷（Hyp）对正常小鼠免疫功能的影响。方法采用碳廓清实验、溶血素实验及淋巴细胞增殖实验,观察Hyp对正常小鼠的非特异性免疫、体液免疫和细胞免疫的影响。结果碳廓清试验,Hyp低剂量组（12．5mg·kg^-1）可显著提高小鼠碳阔清指数k（P〈0．05）,Hyp中、低剂量组（25、12．5mg·kg^-1）可明显提高小鼠吞噬指数α（P〈0．05或P〈0．01）,增强正常小鼠巨噬细胞的吞噬功能;溶血素试验,Hyp高、中、低剂量组（50、25、12．5mg·kg^-1）A值均大于模型组（P〈0．05或P〈0．01）,能明显促进鸡红细胞致敏小鼠溶血素的生成;淋巴细胞增殖实验,Hyp高、中、低剂量组（0．5、0．25、0．125mg·mL^-1）对淋巴细胞增殖均有促进作用（P〈0．01）。结论Hyp对正常小鼠的非特异性免疫、体液免疫和细胞免疫功能具有增强作用。     

HPLC法测定苎麻根中大黄素的含量

目的建立苎麻根中大黄素的含量测定方法。方法采用VP-ODS C18（4.6 mm×250 mm,5μm）色谱柱。以甲醇-0.1%磷酸溶液（80∶20）为流动相;流速为1.0 ml·min-1;检测波长为254 nm。结果苎麻根中的大黄素含量在0.1014~0.5070μg范围内进样量与峰面积的线性关系良好（r=0.9999）;平均回收率为100.11%,RSD为1.11%。结论所建立的方法准确、灵敏、重复性好,可用于苎麻根的质量控制。     

Rhinocerebral mucormycosis: MR manifestations

Magnetic resonance (MR) examinations of three patients with rhinocerebral mucormycosis are reviewed. The clinical course is outlined and the MR characteristics are analyzed in light of the known pathology. The major MR findings include sinus and orbital disease followed by deep facial extension. Involvement of basal portions of the hemispheres, brain stem, and hypothalamus occurred rapidly following ipsilateral facial or orbital invasion in all three cases. Regions of intracerebral inflammation were hyperintense compared with normal parenchyma on T2-weighted and proton density-weighted images. Septic cavernous sinus and internal carotid artery thrombosis was diagnosed by MR in one case. Magnetic resonance demonstrated partial resolution of intracerebral abnormalities that accompanied clinical improvement in the one surviving patient.     

儿童脑多形性黄色星形细胞瘤的MRI分析

目的 :分析儿童期脑多形性黄色星形细胞瘤 (PXA)的MRI表现。方法 :对经手术病理证实的 7例儿童期脑PXA的MRI资料进行回顾性分析 ,研究肿瘤的部位、形态和信号特征。结果 :7例肿瘤均呈囊实性 ,位于脑表浅部位 ,3例边界清楚 ,4例边界欠清楚。肿瘤实质与脑灰质比较在T1WI呈低信号 ,在T2 WI呈混合性高信号 ,增强后肿瘤实性部分和壁结节明显强化 ,3例囊性伴壁结节的肿瘤中 2例囊壁有强化 ,1例无强化。结论 :儿童期脑PXA多起源于脑表浅部位 ,颞叶为最常见部位 ,肿瘤常呈囊实性 ,增强后肿瘤实性部分和壁结节明显强化。     

Chronic cystic lesion of the sacrum: characterisation with diffusion-weighted MR imaging

PURPOSE: Sacral bone remodelling with abnormal dilatation of intervertebral foramina is usually associated with Tarlov cysts but can be caused by slow-growth lesions, which also may present cerebrospinal-fluid (CSF)-like signal or density. We describe three patients with a similar history of lower back pain presenting CSF-like density/signal lesions with extensive sacral bone remodelling who were affected by a Tarlov cyst, an epidermoid cyst and a giant neurofibroma, respectively. MATERIALS AND METHODS: Magnetic resonance imaging (MRI) studies were performed with 1.0-T magnet; axial and sagittal pre- and postcontrast T1-and T2-weighted images were obtained. Moreover, axial and sagittal diffusion-weighted (DWI) echoplanar images were produced, and corresponding apparent diffusion coefficient (ADC) values were calculated. ADC values were measured within the lesions on axial images. RESULTS: All lesions presented a CSF-like signal on conventional MRI. The Tarlov cyst was hypointense on DWI with high ADC values (2,793 s/mm(2)+/-137). The epidermoid cyst proved to be markedly hyperintense on DWI, with reduced ADC values (855 s/mm(2)+/-109). The neurofibroma was isointense on DWI, with ADC values not compatible with CSF (1,467 s/mm(2)+/-130). CONCLUSIONS: DWI and ADC values seem to be able to clearly differentiate Tarlov cysts from slow-growth lesions, allowing for adequate treatment.     

The role of inspiratory muscle training in the management of asthma and exercise-induced bronchoconstriction

Asthma is a pathological condition comprising of a variety of symptoms which affect the ability to function in daily life. Due to the high prevalence of asthma and associated healthcare costs, it is important to identify low-cost alternatives to traditional pharmacotherapy. One of these low cost alternatives is the use of inspiratory muscle training (IMT), which is a technique aimed at increasing the strength and endurance of the diaphragm and accessory muscles of respiration. IMT typically consists of taking voluntary inspirations against a resistive load across the entire range of vital capacity while at rest. In healthy individuals, the most notable benefits of IMT are an increase in diaphragm thickness and strength, a decrease in exertional dyspnea, and a decrease in the oxygen cost of breathing. Due to the presence of expiratory flow limitation in asthma and exercise-induced bronchoconstriction, dynamic lung hyperinflation is common. As a result of varying operational lung volumes, due in part to hyperinflation, the respiratory muscles may operate far from the optimal portion of the length-tension curve, and thus may be forced to operate against a low pulmonary compliance. Therefore, the ability of these muscles to generate tension is reduced, and for any given level of ventilation, the work of breathing is increased as compared to non-asthmatics. Evidence that IMT is an effective treatment for asthma is inconclusive, due to limited data and a wide variation in study methodologies. However, IMT has been shown to decrease dyspnea, increase inspiratory muscle strength, and improve exercise capacity in asthmatic individuals. In order to develop more concrete recommendations regarding IMT as an effective low-cost adjunct in addition to traditional asthma treatments, we recommend that a standard treatment protocol be developed and tested in a placebo-controlled clinical trial with a large representative sample.     

Chronic hepatitis C activity: correlation with lymphadenopathy on MR imaging

OBJECTIVE: To study the MR appearance of lymph nodes in relation to activity of chronic active hepatitis C, we correlated the findings on MR imaging with a histologic grading of the activity level. MATERIALS AND METHODS: Fifty patients with chronic active hepatitis C, who had MR imaging examinations and a related histology report from a liver biopsy obtained within 1 month of the MR imaging were chosen from our radiology database and studied retrospectively. All patients were examined over a 4-year period at a single institution to detect cirrhosis or hepatocellular carcinoma. We divided the 50 patients into the mild, moderate, or severe activity groups, according to their histology reports. Two radiologists, unaware of the histologic classifications, individually reviewed the MR images to observe the perihepatic locations, number, size (defined as the sum of the length-by-width products of the largest three nodes), and intensity of the lymph nodes relative to the spleen. The clinical records of the patients were reviewed to check the results of their liver function tests. The lymph node findings on MR imaging were compared with the histologically confirmed activity level of chronic hepatitis C. RESULTS: Forty-four (88.0%) of 50 patients had perihepatic lymph nodes larger than 5 mm on MR images, including 64.2% (9/14) of the patients with mild activity, 96.3% (26/27) of the patients with moderate activity, and 100% (9/9) of the patients with severe activity (p = 0.0034). The average number +/- the standard deviation (SD) of perihepatic lymph nodes was 2.5 +/- 1.8 in patients with mild activity, 5.6 +/- 2.2 in patients with moderate activity, and 8.3 +/- 3.5 in patients with severe activity (p = 0.0001). The average size (+/- SD) of the lymph nodes was 151.0 +/- 104.9 mm(2) in the mild activity group, 366.8 +/- 143.0 mm(2) in the moderate activity group, and 488.2 +/- 244.8 mm(2) in the severe activity group (p = 0.0001). On fat-saturated fast spin-echo T2-weighted MR images, the average number (+/- SD) of hyperintense nodes was 0.17 +/- 0.25 in the mild activity group, 1.7 +/- 0.80 in the moderate activity group, and 2.4 +/- 0.60 nodes in the severe activity group (p = 0.0001). No relationship between histologic activity and results from liver function tests was found. CONCLUSION: MR imaging depicts perihepatic lymph nodes in most patients with chronic hepatitis C. Lymph node number, size, and hyperintensity were related to the activity of chronic hepatitis C, but the results of liver function tests were not.     

免疫球蛋白含量的检测与分离技术探讨

目的 探讨免疫球蛋白含量的检测与分离技术.方法 选取武警北京总队医院2013-10至2016-10收集的90份免疫球蛋白异常血清,运用单扩法对血清IgG含量进行检测,将90份血清分为3组,每组30份,分别运用单扩法、免疫散射比浊法、免疫透射比浊法对血清IgG、IgA、IgM含量进行检测,然后对3种检测方法测定IgG、IgA、IgM的异常情况、免疫球蛋白含量进行统计分析.结果 单扩法测定IgG、IgA、IgM的异常率分别为22.6％、12.4％、7.9％;免疫散射比浊法测定IgG、IgA、IgM的异常率分别为20.3％、14.0％、9.2％;免疫透射比浊法测定IgG、IgA、IgM的异常率分别为8.0％、1.5％、6.2％.单扩法、免疫透射比浊法测定IgG、IgA、IgM的异常率均显著高于免疫透射比浊法(P＜0.05),但单扩法、免疫散射比浊法测定IgG、IgA、IgM的异常率之间的差异均无统计学意义;单扩法、免疫散射比浊法测定IgA、IgM含量均显著高于免疫透射比浊法(P＜0.05),而免疫散射比浊法测定IgA、IgM含量又均显著高于单扩法(P＜0.05),但3种检测方法测定IgG含量之间的差异均无统计学意义.结论 单扩法、免疫透射比浊法测定免疫球蛋白含量效果较免疫透射比浊法好.     

Comparison of scatter and attenuation correction methods in single photon emission CT--simulation study

Quantitative SPECT requires an accurate and appropriate attenuation correction and scatter correction. This paper compares scatter corrected images combined with attenuation correction. The scatter correction methods used here were the deconvolution method, dual energy window subtraction method, triple energy window method, and dual photopeak window method. The attenuation correction methods used were Sorenson's method, iterative Chang's method, and Bellini's method. The numerical phantoms used were the cold spot, hot spot, star, and MCAT phantom. These correction methods were assessed by using profiles and images, contrast values, and linearity of SPECT values.     

化学-机械祛腐法与传统车针祛腐法在乳牙活髓保存治疗中的效果分析

目的探讨化学-机械祛腐法与传统车针祛腐法对深龋近髓乳磨牙治疗结果的差异。方法选取2007年6月—2009年6月就诊患儿的638颗深龋近髓乳磨牙,分为化学-机械祛腐法和传统车针祛腐法两组,去除腐质后,护髓剂Ca(OH)2间接盖髓,含氟玻璃离子水门汀一次性填充,术后1个月～1年内门诊随诊。结果化学-机械祛腐法去龋活髓保存成功率95.3%;传统车针祛腐法去龋活髓保存成功率89.1%,二者有显著性差异(χ2=8.28,P<0.01)。结论化学-机械祛腐法在深龋近髓乳磨牙的治疗中可以更大程度地保存活髓,从而减少对后继恒牙发育的影响。