蒲黄总黄酮提取物中香蒲新苷及异鼠李素-3-O-新橙皮糖苷的HPLC测定

建立了HPLC法测定蒲黄总黄酮提取物中香蒲新苷(1)及异鼠李素-3-O-新橙皮糖苷(2)的含量.采用Eclipse XDB C18柱,乙腈-0.5%乙酸-甲醇梯度洗脱,检测波长248nm.1和2分别在10～400μg/ml和12.6～504μg/ml范围内呈良好线性关系(r=0.9999),平均回收率分别为98.9%和102.3%,RSD分别为1.66%和2.05%.     

高效液相色谱梯度洗脱法同时测定伤科跌打丸中4种有效成分的含量

目的采用高效液相梯度洗脱法测定伤科跌打丸中异鼠李素-3-O-新橙皮苷、香蒲新苷、升麻素苷和5-O-甲基维斯阿米醇苷的含量。方法 Hypersil C18色谱柱(4.6 mm×200 mm,5μm);流速:0.9 mL·min-1;流动相A为乙腈,流动相B为0.05%磷酸溶液梯度洗脱;检测波长254 nm。结果异鼠李素-3-O-新橙皮苷、香蒲新苷、升麻素苷和5-O-甲基维斯阿米醇苷分别在0.031 2⁰.624 0μg(r=0.999 7)、0.023 80.624 0μg(r=0.999 7)、0.023 8⁰.476 0μg(r=0.999 3)、0.015 80.476 0μg(r=0.999 3)、0.015 8⁰.316 0μg(r=0.999 6)、0.010 20.316 0μg(r=0.999 6)、0.010 2⁰.204 0μg(r=0.999 4)进样量与峰面积线性关系良好,平均加样回收率分别为98.4%、97.7%、98.5%、97.7%,RSD(n=6)分别为1.1%、0.82%、0.89%、0.79%。结论该含量测定方法结果准确、灵敏、重复性好。     

高效液相色谱法测定复方蒲黄片中香蒲新苷与异鼠李素-3-O-新橙皮糖苷含量

目的 建立测定复方蒲黄片中香蒲新苷和异鼠李素-3-O-新橙皮糖苷含量的高效液相色谱法. 方法 采用Luna C18柱(4.6 mm×250 mm,5 μm),以乙腈-0.4%磷酸为流动相进行梯度洗脱,流速0.8 mL.min^-1,柱温30 ℃,检测波长254 nm. 结果香蒲新苷和异鼠李素-3-O-新橙皮糖苷分别在0.029～0.570 mg.mL^-1 和 0.050～1.010 mg.mL^-1浓度范围内有良好线性关系,平均加样回收率分别为98.0%和97.5%,RSD均<2.0%. 结论 该方法简便,快速,准确,重复性好,可用于该制剂的质量控制.     

蒲药灌肠液的质量控制

目的:建立蒲药灌肠液的质量控制方法。方法:采用薄层色谱法对乳香、黄芪甲苷和延胡索乙素进行定性鉴别,采用高效液相色谱法同时测定香蒲新苷和异鼠李素-3-O-新橙皮苷的含量。结果:薄层色谱均检出乳香、黄芪甲苷和延胡索乙素,斑点清晰,专属性强;含量测定中香蒲新苷和异鼠李素-3-O-新橙皮苷的线性范围分别为0.216 0~3.240μg(r=0.999 9,n=6)和0.208 8~3.132μg(r=0.999 8,n=6),加样回收率分别为98.6%(RSD=1.3%,n=6)和98.4%(RSD=1.4%,n=6)。结论:该方法简便可行,结果准确可靠,可用于蒲药灌肠液的质量控制。     

HPLC法同时测定蒲药灌肠液中3个有效成分的含量

摘 要 目的： 建立蒲药灌肠液中香蒲新苷、异鼠李素-3-O-新橙皮苷和延胡索乙素的HPLC含量测定方法。方法: 采用ZORBAX SB-C₁₈色谱柱（250 mm×4.6 mm,5 μm）,以乙腈-0.1%磷酸（三乙胺调节pH至6.0）为流动相,梯度洗脱程序,流速:1.0 ml·min^-1,检测波长为254 nm（0～14 min）和281 nm（14～25 min）,柱温:30 ℃。结果: 香蒲新苷、异鼠李素-3-O-新橙皮苷和延胡索乙素的线性范围分别为19.840～198.400 μg·ml^-1（r=0.999 6）、20.520～205.200 μg·ml^-1（r=0.999 8）和10.040～100.400 μg·ml^-1（r=0.999 7）,回收率分别为98.8%、98.6%和98.9%,RSD分别为1.4%、1.6%和1.3%（n=6）。结论: 该方法灵敏度高,专属性强,可用于蒲药灌肠液的质量控制。     

狭叶香蒲花粉(蒲黄)黄酮类成分的研究

自香蒲科(Typhaceae)植物狭叶香蒲(Typha augustifolia L.)的干燥花粉中分离到五个黄酮醇甙,包括两个黄酮醇-3-三糖甙(Ⅰ,Ⅱ)和三个黄酮醇-3-双糖甙(Ⅲ,Ⅳ,Ⅴ)。其中,化合物Ⅰ是一个新的黄酮醇甙,为本植物的主要成分,经光谱分析(UV,IR.MS;¹HNMR和¹³CNMR)和水解试验确定为异鼠李素-3-0-(2_G-α-L-鼠李糖基)-α-L-鼠李糖(1→6)-β-D-葡萄糖甙,命名为香蒲新甙(typhaneoside,Ⅰ)。其它四种为已知成分。Ⅱ从本属植物中首次发现。     

60Co-γ射线辐照对复方止血胶囊中3种有效成分的影响研究

摘 要 目的：建立HPLC法同时测定复方止血胶囊中3种活性有效成分含量的测定方法,考察60Co γ射线辐照前后活性成分含量的变化。方法: 采用Agilent C18色谱柱 (250 mm×4.6 mm,5 μm),以乙腈 0.5%磷酸溶液（三乙胺调节pH至6.0）为流动相,梯度洗脱程序,检测波长为254 nm(0～35 min)和281 nm(35～55 min), 流速为1.0 ml·min^-1,柱温为35℃。分别选择辐照剂量为5,8,10 kGy对复方止血胶囊进行辐照,比较辐照前后复方止血胶囊中3种活性成分含量的变化。结果:香蒲新苷、异鼠李素 3 O 新橙皮苷和延胡索乙素分别在0.018 0～0.113 0 mg瘙
簚ml^-1、0.020 0～0.120 0 mg瘙
簚ml^-1和0.011 0～0.066 0 mg瘙
簚ml^-1范围内与各自峰面积呈良好的线性关系,平均回收率分别为97.7%、98.7%、99.3%,RSD分别为0.9%、0.9%、0.5%（n=6）;经过5,8,10 kGy辐照后,复方止血胶囊所含的有效成分香蒲新苷、异鼠李素 3 O 新橙皮苷、延胡索乙素均有变化,在8kGy剂量下辐照时,香蒲新苷、异鼠李素 3 O 新橙皮苷辐照前后无统计学意义(P＞0.05),而当剂量增加到10 kGy时,延胡索乙素的含量与辐照前差异显著(P＜0.05)。结论:所建立的复方止血胶囊活性有效成分测定方法回收率高,重复性好,简单实用,分离度良好,可作为复方止血胶囊质控方法。60Co γ射线辐照对复方止血胶囊的灭菌效果显著,在辐照剂量不超过5kGy时,各成分变化不显著,可为复方止血胶囊辐照灭菌手段提供了参考。     

五灵止痛胶囊中异鼠李素-3-O-新橙皮苷的含量测定

目的:采用高效液相色谱法测定五灵止痛胶囊中异鼠李素-3-O-新橙皮苷(C28H32O16)的含量.方法:色谱柱:Hypersill BDS C18 5μm,以乙腈-水(15:85)为流动相,流速1.0m·1min-1,检测波长254nm.结果:异鼠李素-3-O-新橙皮苷进样量在0.2～1.0μg范围内与峰面积具有良好的线性关系,相关系数0.9995,回收率99.72%.结论:本方法操作简便,精密度好,结果准确可靠,可以作为该药品的质量检测标准.     

HPLC梯度洗脱法同时测定镇痛活络酊中4种成分的含量

目的建立同时测定镇痛活络酊中香蒲新苷、异鼠李素-3-O-新橙皮苷、巴西苏木素和(±)原苏木素B含量的高效液相色谱法。方法采用依利特C18柱;流动相为乙腈(A)-0.5%磷酸溶液(B),梯度洗脱;流速:1.3 mL/min;柱温:26℃;检测波长λ_1=254 nm(香蒲新苷及异鼠李素-3-O-新橙皮苷),λ_2=285 nm[巴西苏木素和(±)原苏木素B]。结果香蒲新苷、异鼠李素-3-O-新橙皮苷、巴西苏木素和(±)原苏木素B的线性范围分别为4.62~92.40μg/mL(r=0.999 2)、5.70~114.00μg/mL(r=0.999 6)、8.95~179.00μg/mL(r=0.999 4)、7.79~155.80μg/mL(r=0.999 7);香蒲新苷、异鼠李素-3-O-新橙皮苷、巴西苏木素和(±)原苏木素B的平均加样回收率分别为97.81%、99.16%、97.23%、96.74%,其RSD分别为1.19%、0.84%、1.04%、1.08%。结论所建立的镇痛活络酊样品中,4种成分(香蒲新苷、异鼠李素-3-O-新橙皮苷、巴西苏木素和(±)原苏木素B)的含量测定方法准确、可靠。     

HPLC法测定通便宁片中8种成分及其化学计量学综合评价

目的 建立HPLC法测定通便宁片中咖啡酸、儿茶素、表儿茶素、芹菜素-6,8-二-C-葡萄糖苷、异鼠李素-3-O-β-龙胆二糖苷、番泻苷B、番泻苷A、丁内未利葡萄糖苷,结合化学计量学综合评价产品质量。方法 采用Discovery C18色谱柱（250 mm×4.6 mm,5μm）,流动相0.3%冰醋酸–乙腈,梯度洗脱;检测波长为325 nm(0～13 min检测咖啡酸)、270 nm(13～55 min检测儿茶素、表儿茶素、芹菜素-6,8-二-C-葡萄糖苷、异鼠李素-3-O-β-龙胆二糖苷、番泻苷B、番泻苷A和丁内未利葡萄糖苷);柱温30℃;体积流量1.0 mL/min;进样量10μL。运用聚类分析（CA）、主成分分析（PCA）、正交偏最小二乘判别分析法（OPLS-DA）对测定结果进行综合分析。结果 咖啡酸、儿茶素、表儿茶素、芹菜素-6,8-二-C-葡萄糖苷、异鼠李素-3-O-β-龙胆二糖苷、番泻苷B、番泻苷A、丁内未利葡萄糖苷分别在0.49～12.25、0.36～9.00、1.08～27.00、4.15～103.75、39.47～986.75、43.71～1092.75、29.20～7...     

蒲黄与草蒲黄的质量分析

目的考察蒲黄与草蒲黄之间的质量差异。方法从药材性状、显微鉴别、总灰分检查、醇浸出物测定和含量测定等方面,比较蒲黄与草蒲黄之间的质量差异。结果蒲黄与草蒲黄之间的质量差异较大。结论蒲黄的质量明显优于草蒲黄,商品蒲黄需要综合从多方面对其进行质量控制。     

蒲黄药材及其饮片的质量分析

目的：评价蒲黄药材及饮片的质量。方法：通过对蒲黄药材及饮片的现行法定标准检验和探索性研究检验,综合评价其质量状况。结果：按现行法定标准检验蒲黄及其饮片134批次,不合格率为25.4%;通过探索性研究检验,发现染色、增重和掺假为影响本品质量的主要问题,且有用多种染色剂进行非法染色的情况。结论：蒲黄药材及饮片总体质量可通过法定检验和探索性研究检验予以监测,但其质量问题来源复杂,须从生产、流通、使用各个环节加强监督管理,综合进行质量控制以保障民众用药的安全与有效。     

Characterization, thermal stability studies, and analytical method development of Paromomycin for formulation development

Paromomycin (PM) is an aminoglycoside antibiotic, first isolated in the 1950s, and approved in 2006 for treatment of visceral leishmaniasis. Although isolated six decades back, sufficient information essential for development of pharmaceutical formulation is not available for PM. The purpose of this paper was to determine thermal stability and development of new analytical method for formulation development of PM. PM was characterized by thermoanalytical (DSC, TGA, and HSM) and by spectroscopic (FTIR) techniques and these techniques were used to establish thermal stability of PM after heating PM at 100, 110, 120, and 130 °C for 24 h. Biological activity of these heated samples was also determined by microbiological assay. Subsequently, a simple, rapid and sensitive RP‐HPLC method for quantitative determination of PM was developed using pre‐column derivatization with 9‐fluorenylmethyl chloroformate. The developed method was applied to estimate PM quantitatively in two parenteral dosage forms. PM was successfully characterized by various stated techniques. These techniques indicated stability of PM for heating up to 120 °C for 24 h, but when heated at 130 °C, PM is liable to degradation. This degradation is also observed in microbiological assay where PM lost ～30% of its biological activity when heated at 130 °C for 24 h. New analytical method was developed for PM in the concentration range of 25–200 ng/ml with intra‐day and inter‐day variability of < 2%RSD. Characterization techniques were established and stability of PM was determined successfully. Developed analytical method was found sensitive, accurate, and precise for quantification of PM. Copyright © 2010 John Wiley & Sons, Ltd.     

Effect of alkylation with different sized substituents on thermal stability of lysozyme

The amino groups of hen egg white lysozyme were reductively alkylated by the reaction with aliphatic aldehydes of various chain lengths and with two aldehydes of different steric hindrance at pH 7.5 and 4° for 3 h. About four of the original six lysine residues were modified by the reaction with acetaldehyde, n-butylaldehyde or n-hexylaldehyde. About three lysine residues were 2, 2-dimethylpropylated with trimethy-lacetaldehyde while a single residue was modified with benzaldehyde. The thermal stabilities of these alkylated lysozymes were investigated by differential scanning calorimetry (DSC) at different acidic pH values. Alkylation thermally destabilized the proteins, depending not only on the extent of modification but also on the size of the substituent. The alkylated derivatives were 8–19kJ/mol less stable than native lysozyme at 25° and pH 3.0. The temperature dependences of the activities of the alkylated lysozymes against ethylene glycol chitin indicated that the orders of the optimum temperatures and the maximum activities were exactly the same as the order of the thermal stabilities.     

Preparation method and stability of ellagic acid-rich pomegranate fruit peel extract

A simple one-step purification using liquid–liquid extraction for preparing pomegranate peel extract rich in ellagic acid has been demonstrated. The method involved partitioning of the 10% v/v water in methanol extract of pomegranate peel between ethyl acetate and 2% aqueous acetic acid. This method was capable of increasing the ellagic acid content of the extract from 7.06% to 13.63% w/w. Moreover, the antioxidant activity of the extract evaluated by 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging assay was also increased (ED₅₀ from 38.21 to 14.91?μg/mL). Stability evaluations of the ellagic acid-rich pomegranate peel extract in several conditions through a period of four months found that the extracts were stable either kept under light or protected from light. The extracts were also stable under 4° ± 2°C, 30° ± 2°C and accelerated conditions at 45°C with 75% relative humidity. However, study on the effect of pH on stability of the extract in the form of solution revealed that the extract was not stable in all tested pH (5.5, 7 and 8). These results indicated that the ellagic acid-rich pomegranate peel extract was stable when it was kept as dried powder, but it was not stable in any aqueous solution.     

4-色满酮Mannich碱类化合物的合成及其水溶液的热稳定性研究

目的设计合成一些 4 色满酮Mannich类化合物 ,并且考察其水溶液的稳定性。方法以取代的 4 色满酮为原料 ,经过Mannich反应合成 4 色满酮Mannich碱类化合物 ,并利用高效液相色谱法测定所合成的 4 色满酮Mannich碱类化合物的水溶液的稳定性。结果合成 3种 4 色满酮Mannich碱类化合物 ,并经元素分析 ,红外光谱 ,核磁共振氢谱确认了化合物结构 ,其水溶液在室温和 (37± 1)℃时 2 4h内均没有显著分解。     

磺胺嘧啶银乳膏含量测定方法的优化和极端环境下的稳定性考察

目的 优化磺胺嘧啶银乳膏中磺胺嘧啶银的含量测定方法,并考察其在高温、高湿、高盐环境下的稳定性.方法 采用反相高效液相色谱法,选用Agilent ZORBAX SB-C18色谱柱(4.6 mm×150 mm,5μm),流动相:乙腈-0.1％磷酸(8:92,V/V),流速1.0 ml/min,柱温30℃,检测波长254 n...     

Preparation of high thermal stability polysulfone microcapsules containing lubricant oil and its tribological properties of epoxy composites

Polysulfone (PSF) microcapsules containing lubricant oil have been successfully prepared using solvent evaporation method. The results show that lubricant oil was successfully encapsulated and the encapsulation capacity of about 56.0?wt.% was achieved. The uniform microcapsules have nearly spherical shape and quite smooth outer surface. The mean diameter is approximately 156 and 169?μm by using different dispersant solutions. The wall material is porous in structure with wall thickness of about 20?μm. The initial decomposition temperature of PSF is 480?°C. It is higher than traditional poly(urea-formaldehyde) (PUF) and poly(melamine-formaldehyde) (PMF) wall materials with 245?°C and 260?°C initial decomposition temperature, respectively. High thermal stability of PSF microcapsules can be considered as additives in high temperature resistant polymer materials. The frictional coefficient and wear rate of epoxy composites decreased significantly by incorporating microcapsules containing lubricant oil into epoxy. When the concentration of microcapsules was 25?wt.%, the frictional coefficient and specific wear rate were reduced by 2.3 and 18.3 times, respectively, as compared to the neat epoxy.     

优选复方替硝唑霜基质及稳定性

目的：优选复方替硝唑霜的基质组成及对物理稳定性进行考察。方法：用正交试验法,以液体石蜡、十六醇、单甘酯、凡士林的配比为因素,在3个水平上进行拟合,以乳剂在45℃的分层时间及外观为指标,用L9（3^4)表进行实验。结果：最优基质组成为：液体石蜡5%,十六醇15%,单甘酯2%,凡士林10%。结论：按此比例制备的复方替硝唑霜符合中国药典2000年版的规定。