肾八味胶囊中大黄的测定

目的对肾八味胶囊中的大黄进行鉴别和含量测定.方法采用薄层色谱(TLC)法对处方中的大黄进行鉴别,并采用高效液相色谱(HPLC)法测定其含量.结果TLC鉴别大黄素、大黄酚斑点清晰.HPLC定量分析中,大黄素的线性范围为1.1～22.0 mg·L-1,r=0.999 2;平均回收率为96.7%,RSD为2.0%(n=5).大黄酚的线性范围1.2～24.0 mg·L-1,r=0.999 7;平均回收率为101.6%,RSD为1.9%(n=5).结论薄层鉴别大黄素、大黄酚,方法专属、斑点清晰;HPLC法测定其含量,方法准确,重复性好.     

小儿导赤片质量控制方法改进研究

目的建立小儿导赤片中大黄、栀子含量测定的高效液相色谱(HPLC)法及栀子的薄层色谱(TLC)鉴别方法。方法用TLC法和HPLC法对小儿导赤片中大黄及栀子进行定性、定量分析。结果 TLC色谱中,栀子苷和栀子对照药材斑点清晰。大黄素质量浓度的线性范围为8.096～104.48μg/mL(r=0.999 9),平均回收率为98.01%(RSD为1.25%);大黄酚质量浓度的线性范围为10.83～112.23μg/mL,r=0.999 9;芦荟大黄素的线性范围为8.12～89.90μg/mL,r=0.999 8;大黄酸的线性范围为9.96～89.48μg/mL,r=0.999 8;大黄素甲醚的线性范围为8.896～54.44μg/mL,r=0.999 7;栀子苷的线性范围为6.771～141.48μg/mL(r=1.000 0),平均回收率为99.04%(RSD为1.20)。结论定性鉴别方法专属、斑点清晰;含量测定方法可靠,重现性好。     

厚术胶囊质量标准研究

目的:建立厚术胶囊的质量标准。方法:采用薄层色谱(TLC)法对方中苍术、三七、白芍和山楂药材进行定性鉴别;采用高效液相色谱法测定厚朴中厚朴酚、和厚朴酚的含量。结果:TLC斑点清晰,阴性对照无干扰。厚朴酚与和厚朴酚的进样量分别在0.080～0.400μg(r=0.9999)、0.048～0.240μg(r=0.9999)范围内与各自峰面积积分值呈良好的线性关系;平均回收率分别为98.42%、98.34%,RSD分别为0.63%、0.90%(n=6)。结论:所建标准可有效控制厚术胶囊的质量。     

利胆片中药材的鉴别及大黄的含量测定

目的:提高利胆片的质量标准.方法:采用薄层色谱(TLC)法鉴别金银花、黄芩、知母及白芍,用高效液相色谱(HPLC)法测定方中大黄的含量.结果:TLC鉴别斑点明显.含量测定大黄素0.01064～0.3192 μg、大黄酚0.02586～0.7758 μg,进样量与峰面积线性关系良好.平均加样回收率大黄素为99.80%,RSD=0.78%(n=6);大黄酚为99.72%,RSD=1.18%(n=6).结论:建立的TLC鉴别和HPLC含量测定方法专属性强、重复性好,可用于利胆片的质量控制.     

HPLC法测定肾康丸中大黄酚、大黄素的含量

目的:建立肾康丸中大黄酚、大黄素的含量测定方法。方法:采用HPLC法,色谱柱为Diamonsi C18(250 mm×4.6 mm,5μm),流动相为乙腈-甲醇-0.1%磷酸溶液(42∶23∶35),流速为1.0 ml.min-1,检测波长为254 nm,进样量10μl。结果:大黄酚在9.38～150.00μg.ml-1(r=1.000 0),大黄素在3.31～53.00μg.ml-1(r=1.000 0)之间线性关系良好,其平均加样回收率大黄酚为99.83%,RSD为0.75%;大黄素为99.73%,RSD为0.34%。结论:此法简便,结果准确、灵敏,可用于肾康丸的含量测定。     

基于多指标成分定量的复方蛭甲软肝颗粒质量标准研究

摘要：目的:基于多指标成分TLC鉴别及HPLC含量测定全面控制蛭甲软肝颗粒质量。方法:采用TLC色谱法对方中水蛭、丹参、大黄、三七进行鉴别;采用HPLC对防己、夏枯草、丹参、淫羊藿、大黄中的主要活性成分粉防己碱、迷迭香酸、丹酚酸B、淫羊藿苷、大黄酸、大黄素的含量进行测定。结果:TLC鉴别方法斑点清晰,专属性强,无阴性干扰;HPLC测定结果表明粉防己碱、迷迭香酸、丹酚酸B、大黄酸、大黄素的线性范围分别为9.30～298.80μg·ml-1（r=0.999 7）、2.30～73.10μg·ml-1（r=0.999 5）、30.50～975.70μg·ml-1（r=0.999 2）、1.50～47.50μg·ml-1（r=0.999 3）、4.50～145.00μg·ml-1（r=0.999 5）、4.10～130.00μg·ml-1（r=0.999 6）;平均加样回收率分别为101.88%（RSD=1.69%）,100.96%（RSD=1.47%）,100.13%（RSD=1.79%）,102.45%（RSD=1.72%）,102.78%（RSD=1.45%）,101.03%（RSD=1.70%）（n=6）。结论:本研究建立多指标成分TlC鉴别及HPlC含量测定方法稳定性好,专属性强,准确度高,可作为蛭甲软肝颗粒的质量控制标准。     

四川产亚大黄的鉴别及其大黄素、大黄酚的测定

目的鉴别四川产亚大黄,并测定其大黄素、大黄酚的含量。方法采用显微鉴别、TLC法对药材进行鉴别,用HPLC法测定大黄素、大黄酚的含量。结果 TLC法鉴别亚大黄的专属性强;建立了HPLC测定疏枝大黄中大黄素、大黄酚含量的方法。结论所用方法操作简便、结果准确、重复性好,可用于四川产亚大黄的质量控制。     

五味化痔胶囊快速薄层鉴别与定量测定研究

目的:建立简便、快捷的五味化痔胶囊质量控制方法。方法:用TLC法鉴别大黄、地龙与人工牛黄,用HPLC法测定了胶囊中总的与游离的大黄酚、大黄素。结果:薄层鉴别斑点清晰,阴性无干扰。方法学研究表明,大黄酚进样量在0.046 8～0.819μg,大黄素的进样量在0.019 92～0.996μg,分别与峰面积呈良好的线性关系。大黄酚的平均回收率为99.77%(n=9),RSD为1.92%;大黄素的平均回收率为99.57%(n=9),RSD为1.53%。结论:方法简便、快捷、实用,能保证五味化痔胶囊的有效性与安全性。     

济坤丸质量标准研究

目的：建立济坤丸中木香、牡丹皮及延胡索的薄层色谱（TLC）鉴别及厚朴的高效液相色谱（HPLC）含量测定方法。方法：采用TLC法，分别以三氯甲烷-环己烷（5：1）、环己烷-乙酸乙酯（3：1）及正己烷-三氯甲烷-甲醇（15：10：1）为展开剂，建立木香、牡丹皮及延胡索的鉴别方法；采用Agilent TC—C18（250mm×4．6mm，5μm）色谱柱，甲醇-异丙醇-水（45：20：35）为流动相，检测波长为294nm。结果：薄层鉴别中样品色谱斑点清晰，分离较好。含量测定和厚朴酚在15．15—3030μg、厚朴酚在15．10～3050μg范围内呈良好线性关系（r=0．9999）；和厚朴酚平均回收率为97．78％，RSD为1．4％；厚朴酚平均回收率为100．19％，RSD为1．1％。结论：本实验方法简便、准确、可靠。     

大黄滴眼液质量标准研究

目的建立大黄滴眼液的质量标准。方法选用TLC法鉴别制剂中大黄有效成分大黄酸;进行pH等项目的检查;选用HPLC法测定芦荟大黄素、大黄酸、大黄素和大黄酚的含量。结果薄层色谱斑点清晰,分离度好。芦荟大黄素在2.532~50.646μg·mL-1范围内呈良好的线性关系(r=1.000 0),平均回收率为91.8%,RSD为0.79%。大黄酸在3.764~75.280μg·mL-1范围内呈良好的线性关系(r=1.000 0),平均回收率为99.4%,RSD为1.46%。大黄素在2.608~52.160μg·mL-1范围内呈良好的线性关系(r=1.000 0),平均回收率为92.4%,RSD为0.87%。大黄酚在2.499~49.989μg·mL-1范围内呈良好的线性关系(r=0.999 9),平均回收率为92.6%,RSD为0.85%。结论该方法操作简单,结果可靠,可用于大黄滴眼液的质量控制。     

Antagonism of morphine by beta-melanocyte-stimulating hormone and by tetracosactin

Using the decerebrate—spinal Lloyd preparation morphine depressed evoked mono- and polysynaptic reflex activity, β-melanocyte-stimulating hormone enhanced monosynaptic reflex activity, and tetracosactin had no effect. When morphine injection was preceded either by β-melanocyte-stimulating hormone or by tetracosactin a statistically significant depression was not observed. The stimulant actions of β-melanocyte-stimulating hormone did not appear to account for its capacity to antagonize morphine. The fall of blood pressure which follows the administration of morphine in this preparation was not antagonized by the prior administration of either polypeptide.     

冠舒注射液的薄层色谱鉴别及含量测定

报道了冠舒注射液中葛根和元胡的薄层色谱鉴别结果，方法简便。并用分光光度法对其总黄酮的含量进行了测定，以便控制产品质量，结果可靠、重现性好．三批样品含量分别为８．７８３、７．９０６和８．１３４ｍｇ／ｍｌ。     

Synergism by caffeine and by cocaine of the motor control deficit produced by midazolam

To evaluate the effects of caffeine and cocaine on the impairment of discriminative motor control produced by midazolam, rats were trained to hold a force transducer operated with a paw so that it remained between upper and lower limits of a force band for a continuous 1.5-s period to deliver each food pellet. Acute doses of 3 mg/kg midazolam SC impaired motor performance. Except for one animal, caffeine (10-40 mg/kg IP) had little or no effect on performance, while cocaine (3.75-22.5 mg/kg IP) produced dose-related impairment. When each dose of caffeine was combined with 3 mg/kg midazolam, a marked synergism in motor performance impairment occurred. Cocaine plus midazolam produced mainly an additive synergism. The conspicuous synergistic action of caffeine on the motor control deficit produced by midazolam contrasts with the typical antagonism found between the benzodiazepines and methylxanthines when performance is evaluated by psychomotor tests not requiring fine motor control.     

A comparison of granules prepared by pan granulation and by massing and screening

Granules of lactose and calcium phosphate were prepared by pan granulation and by massing and screening. Capillary forces and the gentle action of tumbling in the pan were inadequate to compact the fine cohesive calcium phosphate but were highly effective with the less cohesive lactose where the absence of shear gave very high densification. Whereas massing and screening provided the necessary forces for consolidating calcium phosphate, with lactose a more open structure resulted which further dilated during screening. Increase in both moisture content and time of mixing increased granule density but the degree varied with both method and material as did granule shape, strength and compressibility.     

奥利司他的制备液相色谱纯化及其UPLC法测定

建立了制备液相色谱法纯化奥利司他粗品。取3%奥利司他粗品溶液上样,以89%乙腈溶液为流动相进行洗脱,检测波长195 nm,分段收集洗脱液。采用UPLC法测定洗脱液中的奥利司他,使用Acquity BEH C18色谱柱,流动相为81%乙腈溶液,检测波长195 nm。奥利司他在0.2～1 mg/ml范围内线性关系良好,回收率为98.8%,RSD为0.16%。     

重组人白细胞介素-15包涵体离子交换柱复性与稀释复性的比较

目的比较重组人白细胞介素-15 (rhIL-15 )包涵体蛋白稀释复性法与离子交换柱复性法的效果。方法采用离子交换柱吸附变性包涵体蛋白,用含有复性剂的洗脱液洗脱复性,所得蛋白质比活和稀释复性法所得比活比较。结果两种方法所得目的蛋白质比活相近,但离子交换柱复性法目的蛋白质回收率高,试剂消耗少。结论对于rhIL-15包涵体,离子交换柱复性法用于生产,可大幅降低生产成本     

电化学发光法测定HBV标志物与荧光定量PCR-HBV-DNA结果的分析比较

目的探讨HBV标志物与HBV-DNA的相关性,更加准确地了解患者HBV感染、病毒复制和传染性情况,为临床制定合理的治疗方案、疗效观察和预后评估提供依据。方法用电化学发光法测定HBV标志物,用实时荧光定量PCR方法检测HBV-DNA。结果 HBV标志物模式1～5均有HBV-DNA阳性检出,其中模式4的检出率最高(81.7%),而且DNA含量也最高;模式6～9均为DNA阴性。在乙肝五项指标中,HBeAg的定量结果与HBV-DNA含量相关性最大(r=0.713)。结论 HBV标志物和HBV-DNA既相关又有所不同,应将两者结合起来并相互补充才能更好的反映患者HBV病毒复制和传染性情况。     

Depletion of pituitary corticotrophin by reserpine and by a nitrogen mustard

A single intraperitoneal injection of reserpine (2.5 mg./kg.) into rats produced a fall in the corticotrophin concentration of the pituitary to 30% of the resting value; recovery was not far from complete at 40 hr. A single injection of a nitrogen mustard caused an even greater loss of pituitary corticotrophin; 24 hr. after the injection the concentration was 10% of the resting value. There is no reason to assume that the effect of reserpine is due to an interference with storage of ACTH in the tissue and is not simply due to the fact that the drug acts as a stressing agent. The shape of the curve representing the fall in pituitary ACTH during the early phases of a sudden stress may be very similar to that of the fall in adrenal ascorbic acid produced by the released ACTH. This suggests that, under these circumstances, resynthesis is slow and the diminishing stores of ACTH in the pituitary reflect mainly the release of the hormone.