双水相体系萃取分离-高效液相色谱法测定蛇床子中蛇床子素的研究

目的利用双水相体系分离纯化中药蛇床子中有效成分蛇床子素。方法采用非离子表面活性剂TritonX-114/（NH4）2SO4双水相体系萃取蛇床子中蛇床子素,考察了TritonX-114浓度、（NH4）2SO4盐浓度、萃取温度和pH值等因素对蛇床子素萃取率的影响,并建立了高效液相色谱法测定萃取液中蛇床子素含量的分析方法。结果蛇床子素在TritonX-114浓度为1.0%,（NH4）2SO4浓度为0.8mol/L,pH值为7.0和水浴温度为45℃萃取条件下的萃取率为98.2%。RSD≤4.3%（n=6）,样品加样回收率为97.2%。结论本文方法所形成双水相体系,操作简便,萃取率高,方法重复性好,可适用于分离蛇床子素。     

Triton X-100及四乙基碘化铵存在下的Lowry蛋白定量法

含Triton X-100及TEA的蛋白质溶液以TCA沉淀去除了TEA,由于Folin试剂的含量较高,当Triton X-100浓度在1%以下时可以定量蛋白质,灵敏度不降低。     

HPLC法测定脊痛宁胶囊中蛇床子素的含量

目的建立脊痛宁胶囊中蛇床子素的含量测定方法。方法 HPLC法,色谱柱：Diamonsil（R）C18（250 mm×4.6 mm,5μm）;流动相：甲醇-水（68∶32）;流速：1.0 ml·min-1;检测波长：322 nm;柱温：40℃。结果蛇床子素在7.52~75.2μg·ml-1范围内线性关系良好,r=0.9999;回收率为101.30%,RSD为0.15%。结论本方法简便、准确,专属性强,测定结果重复性好,可用于脊痛宁中蛇床子素的质量控制。     

HPLC法同时测定紫果西番莲叶提取物异荭草素与荭草素的含量

目的建立紫果西番莲叶提取物中异荭草素和荭草素的含量测定方法。方法采用HPLC法。Inertsil C18色谱柱（4.6mm×250mm,5μm）;流动相：水-四氢呋喃-异丙醇-乙腈（87∶8∶2∶3）;柱温：30℃,流速：1mL/min;检测波长：360nm。结果异荭草素、荭草素回归方程：Y=2.901×10^4X-188.1,r=0.999 8;Y=1.824×10^4X-228.83,r=0.999 5;线性范围分别为0.012～0.602、0.009～0.451mg.mL^-1。平均回收率分别为100.09%、98.66%,RSD分别为2.10%、1.81%。结论HPLC法测定紫果西番莲叶提取物中异荭草素和荭草素的含量,专属性强、精密度好、操作简单、准确性高。     

脑活素对大鼠及小鼠缺氧的保护作用

目的：观察脑活素对小鼠及大鼠胚脑组织细胞缺氧时的保护作用。方法：用ＴＢＡ微量法测量小鼠脑组织中过氧化脂质的含量;按邹氏法检测及观察培养大鼠胚鼠脑细胞存活状况,计算存活率。结果：脑活素组中小鼠脑组织匀浆过氧化脂质含量及胚鼠脑细胞存活率均较对照组有显著性差异（前者Ｐ＜ ０．０１;后者Ｐ＜ ０．０５） 。结论：脑活素具有明显的抑制自由基产生,提高脑组织细胞抗缺氧能力,从而具有保护脑细胞的作用。     

HPLC法测定感冒清热颗粒中欧前胡素含量

目的建立HPLC法测定感冒清热颗粒中欧前胡素含量的方法,同时对6家不同企业生产的产品进行质量比对。方法采用HPLC法欧前胡素含量测定条件：色谱柱：Diamonsil（R）C18（250 mm×4.6 mm,5μm）,流动相：乙腈-水（49.5∶50.5）,检测波长：300 nm,流速：1.0 ml·min-1。,柱温：35℃;葛根素含量测定方法参照《中国药典》。结果欧前胡素线性范围为0.2955～11.82μg·ml-1（r=0.9999）,平均回收率为99.47%,RSD为0.69%（n=6）;不同企业生产的产品质量有差异,葛根素的含量以每袋计为12.20～24.00 mg。结论 HPLC测定欧前胡素的方法简便,准确,重复性好,可有效控制该制剂的质量。     

氮酮对蛇床子素体外经皮渗透的研究

目的 研究渗透促进剂氮酮对蛇床子素的体外经皮渗透的影响。方法将蛇床子有效部位制成饱和生理氯化钠溶液,采用Valia-Chien扩散池,考察不同浓度的氮酮对蛇床子素经离体鼠皮渗透的影响。结果不同浓度的氮酮对蛇床子素的透皮吸收均有促进作用,5％氮酮对蛇床子素的透皮吸收的促进作用最佳。结论氮酮的作用机理主要为改变角质层的通透性,减低了药物经皮肤渗透的阻力,提高了药物在皮肤角质层的扩散系数。     

HPLC法测定亮菌甲素注射液的含量及有关物质

目的：建立测定亮菌甲素注射液含量有关物质的方法.方法：以甲醇0.1 mol/L乙醇溶液（50∶50）为流动相,检测波长368 nm,流速为1.0 ml/min,采用高效液相色谱法（HPLC）法测定亮菌甲素注射液含量及有关物质.结果：亮菌甲素胶囊在浓度为20～250 μg/ml范围内有良好的线性关系,相关系数为0.9999,平均加样回收率为101.23%,RSD为1.45%.结论：本方法操作简单、快速、准确,可用于亮菌甲素注射液中亮菌甲素的有关物质的检测和含量测定.     

HPLC法测定通络止痛散中血竭素的含量

目的建立通络止痛散中血竭素的HPLC测定方法。方法色谱柱为Agilent ZORBAX SB-C18（4.6 mm×150mm,5μm）,柱温为35℃;流动相为乙腈-0.05 mol.L-1磷酸二氢钠溶液（45∶55）,流速为1 ml.min-1;检测波长480 nm。结果血竭素保留时间约为8 min,与相邻峰的分离度大于1.5。以峰面积对进样浓度线性回归,回归方程为Y=0.032 71 X-1.026,r=0.9999,线性范围为17.43～348.6μg.ml-1,加样回收率为98.9%,RSD为2.0%。结论本方法操作简便,测定结果准确可靠,可用于通络止痛散中血竭素的含量测定。     

高效液相色谱法测定抗痤霜中丹参酮ⅡA的含量

目的建立抗痤霜中丹参酮ⅡA含量的HPLC测定法。方法色谱条件以Kromsil-C18(4.6 mm×150 mm)色谱柱,流动相为甲醇-水(80∶20),流速1 ml.min-1,检测波长270 nm。结果本法回归方程为Y=20871.2X-215.2,r=0.9994,线性范围0.0105~0.105μg/ml,平均回收率为97.64%,日内误差RSD=0.25%(n=5)日间误差RSD=0.65%(n=5)。结论建立的HPLC法测定抗痤霜中丹参酮ⅡA的含量,简便、准确、可靠。     

A complete remote-control system for reliable preparation of [18F]altanserin.

A complete remote control system was constructed for production of the PET 5-HT2A ligand [18F]altanserin by nitro-for-fluoro exchange. Comparing with published methods, the key features include (1) conducting azeotropic distillation and nucleophilic displacement in an open vessel heated by a commercial microwave oven; (2) purifying the product by a single HPLC procedure and (3) removing HPLC solvent by solid phase extraction. The preparation took 114 min with 23% yield and high quality.     

Pseudo-continuous arterial spin labeling at very high magnetic field (11.75 T) for high-resolution mouse brain perfusion imaging

With the increasing number of transgenic mouse models of human brain diseases, there is a need for a sensitive method that allows assessing quantitative whole brain perfusion within a reasonable scan time. Arterial spin labeling (ASL), an MRI technique that permits the noninvasive quantification of cerebral blood flow, has been used to assess rodents brain perfusion. For mice, the reported experiments performed with continuous or pulsed ASL were challenged by poor multislice capability, limited sensitivity, or quantification issues. Here, the recently proposed pseudo-continuous ASL strategy, which has shown great promise for human studies, was investigated for mouse brain perfusion imaging at 11.75 T. Pseudo-continuous ASL was experimentally optimized and compared with a standard flow-sensitive alternating inversion recovery sequence for sensitivity, robustness, absolute quantification, and multislice imaging capability. A sensitivity gain up to 40% and clear advantages for multislice imaging are obtained with pseudo-continuous ASL.     

Automatic brain tissue extraction method using erosion-dilation treatment (BREED) from three-dimensional magnetic resonance imaging T1-weighted data

To improve the efficiency of brain image analysis, we propose a full-automatic method for extracting brain tissue from three-dimensional magnetic resonance imaging of T1-weighted data on the human head (brain tissue extraction method using erosion-dilation treatment [BREED]). The extraction processing is realized by combining signal intensity thresholding by means of the discriminant analysis method and an erosion-dilation treatment of the image. The accuracy of BREED is evaluated using both simulated and subject data. BREED can extract brain tissues with high accuracy (approximately 97%) for either simulated or subject data.     

高效液相色谱法测定茜草双酯固体分散体中茜草双酯的含量

目的建立茜草双酯固体分散体中茜草双酯含量的测定方法。方法采用高效液相色谱法：色谱柱为Eurospher 100-5 C18色谱柱（250mm×4．6mm,5μm）;流动相为甲醇-水（80：20）;流速：1．0mL／min;检测波长：264nm。结果茜草双酯在20．0～100．0μg·mL^-1浓度范围内线性关系良好（r=0．9998）,平均回收率为100．25％,RSD为1．13％。结论本方法专属性好,灵敏、可靠,适用于茜草双酯类制剂药物浓度的检测。     

地黄中寡糖的提取分离工艺研究

目的研究地黄(Rehmannia glutinosa)中寡糖的提取分离工艺。方法建立水苏糖的HPLC测定法;以水苏糖含量为指标,采用正交试验优化地黄水提取物的提取工艺,对水提物进一步用离子交换树脂进一步纯化,再进行活性炭柱层析,以不同浓度梯度乙醇洗脱,分得寡糖的不同部位。结果地黄水提取的最佳工艺为A283C2,即溶剂(水)体积lO倍,提取3次,每次提取1h。水提物经活性炭柱层析得到4个部位,部位Ⅰ～Ⅳ,其中部位Ⅱ及部位Ⅲ中水苏糖的含量分别为20．99％及60．5l％。结论地黄水提取的较佳工艺条件为A283C2,活性炭柱层析可以较好地将地黄中寡糖进行分离,其中水苏糖的HPLC测定法简便、稳定、可靠。     

大孔吸附树脂对半枝莲中黄酮类成分的分离研究

目的以半枝莲中黄酮类成分为分离对象,进行大孔树脂分离工艺优化和分离研究。方法采用溶剂提取法对半枝莲中有效成分进行提取,以其总黄酮的含量为指标,比较4种不同种类大孔树脂(D1400,HPD-100,D101,NKA-2)的吸附性能。并选择吸附性能最优的大孔树脂分离半枝莲中的黄酮类组分,结合HPLC进行分析检测。结果采用70%乙醇水溶液提取(药材溶剂比为1∶8),得到理想的出膏率11.67%(g/g)。UV法测定结果表明,半枝莲提取物中黄酮类成分含量较高18.34%(mg/g)。D101树脂对总黄酮的吸附率最高52.9%(mg/mg)。结论半枝莲中黄酮类成分含量较高,采用D101型大孔树脂分离能够达到理想的吸附效果,总黄酮成分主要集中在大孔树脂分离的20%乙醇水溶液洗脱组分中。     

HPLC法测定兔血浆中茜草双酯的药物浓度

目的建立兔血浆中茜草双酯的血药浓度测定方法。方法采用HPLC法:Eurospher100-5 C18色谱柱(250 mm×4.6 mm,5μm);流动相为磷酸(0.05 mol/L,二乙胺调pH值至5)-乙腈(30∶70);流速为1.0 ml/min;检测波长为264 nm。结果茜草双酯在0.084～20.08μg/ml浓度范围内线性关系良好;低,中,高浓度的平均回收率分别为:86.9%、89.3%、94.2%。结论该法简便,灵敏,可靠,可用于茜草双酯血药浓度检测。     

A simplified method to determine [99mTc]TRODAT-1 in human plasma

[99mTc]TRODAT-1 is a useful imaging agent in evaluating changes in presynaptic dopamine transporters (DAT) for Parkinson's disease and other central nervous system (CNS) neurodegenerative diseases, for which a reduction of dopamine neurons is indicated. As part of an effort to establish a quantitative single-photon emission tomography (SPECT) procedure for imaging CNS DAT, measurement of nonmetabolized [99mTc]TRODAT-1 in human plasma was investigated. After an intravenous injection of [99mTc]TRODAT-1, there are three possible radioactive components in human plasma: hydrophilic compounds (pertechnetate, etc.), lipophilic metabolite(s), and unchanged [99mTc]TRODAT-1. Based on the differences in lipophilicity of [99mTc]TRODAT-1 and its lipophilic metabolite [99mTc]BAT, a new quantitative method for measuring [99mTc]TRODAT-1 with a simple solvent extraction method was developed. Various organic solvents or mixtures of solvents were tested, among which cyclohexane gave the best extraction yield for [99mTc]TRODAT-1 (76.06 +/- 3.32%) with a low extraction for [99mTc]BAT (2.43 +/- 0.82%). Extractions of [99mTc]TRODAT-1 and [99mTc]BAT mixtures in different predetermined ratios to simulate the actual human plasma samples with cyclohexane from phosphate buffer (5 mM, pH 8.0) were evaluated. The experimentally obtained ratios were in good agreement with the theoretical ratios. To investigate further the possibility of replacing the previously established high performance liquid chromatography (HPLC) method with the new solvent extraction method for the clinical application, both HPLC and extraction methods were used side by side to determine the unchanged [99mTc]TRODAT-1 in human plasma samples during [99mTc]TRODAT-1/SPECT imaging studies. The results from four human subjects showed that both methods consistently produced similar values for unchanged [99mTc]TRODAT-1 in the plasma samples. This improved solvent extraction method provides an easy and reliable technique to quantify unchanged [99mTc]TRODAT-1 in human plasma, thus making the clinical application of this agent readily available for quantitation of the DAT binding sites in the brain by SPECT imaging.