高效液相色谱法同时测定不同产地莪术饮片中5种倍半萜类成分的含量

目的:建立HPLC法同时测定不同产地莪术中莪术二酮、莪术醇、吉玛酮、呋喃二烯、β-榄香烯等5种倍半萜类成分的含量。方法:采用Kromasil C18柱(4.6mm×250mm,5μm);流动相:乙腈(A)-水(B),梯度洗脱(0～35min,45%A→70%A;35～40min,70%A→90%A;40～60min,90%A→95%A),流速1.0mL·min-1;检测波长214nm;柱温25℃。结果:莪术二酮、莪术醇、吉玛酮、呋喃二烯、β-榄香烯分别在27.88～278.8,20.42～204.2,3.475～34.75,5.380～53.80,10.12～101.2μg·mL-1范围内线性关系良好,r≥0.999 6。平均加样回收率(RSD)分别为97.36%(1.85%),97.96%(2.30%),97.47%(2.02%),98.10%(2.38%),98.94%(2.01%)。结论:本方法操作简便、准确可靠,适用于莪术中5种倍半萜类成分的定量分析。     

温郁金醋制前后5种成分含量变化考察

摘要：目的:比较温郁金醋制前后5种成分含量变化。方法:采用HPLC法对温郁金和醋温郁金中的莪术二酮、吉马酮、莪术醇、β-榄香烯、姜黄素5种成分进行定量分析。结果:莪术二酮、吉马酮、莪术醇、β-榄香烯、姜黄素5种成分能够良好分离,线性范围分别为2.506～20.050μg·ml-1（r=0.999 5）、0.919～7.355μg·ml-1（r=0.999 6）、0.964～7.714μg·ml-1（r=0.999 7）、0.927～7.416μg·ml-1（r=0.999 4）、1.123～8.982μg·ml-1（r=0.999 3）;平均加样回收率分别为99.59%（RSD=0.95%）,98.84%（RSD=0.91%）,99.41%（RSD=1.19%）,98.72%（RSD=0.79%）,98.94%（RSD=1.06%）（n=6）。温郁金经醋制后莪术二酮及吉马酮的含量显著降低（P<0.05）,莪术醇和β-榄香烯的含量则有所增加,而姜黄素含量无明显变化,5-羟甲基糠醛为炮制后新增加的成分。结论:基于HPLC法对温郁金和醋温郁金中5种成分进行定量分析,为进一步对温郁金炮制前后的质量变化和药效物质基础提供参考依据。     

莪术单煎及与三棱合煎后挥发油中有效成分煎出率的比较研究

目的:研究莪术与三棱配伍前后莪术挥发油中4种有效成分的煎出率变化,为揭示莪术与三棱配伍的作用机制提供参考。方法:采用高效液相色谱法同时测定莪术单煎及与三棱合煎后挥发油中4种有效成分(莪术二酮、莪术醇、吉马酮、β-榄香烯)的含量,并对各成分的煎出率进行比较。结果:与莪术单煎比较,合煎后挥发油中莪术二酮、莪术醇、吉马酮的煎出量差异具有统计学意义(P<0.05),β-榄香烯的煎出率差异无统计学意义(P>0.05)。结论:莪术与三棱配伍合煎后可有效增加其挥发油中有效成分莪术二酮、莪术醇和吉马酮的溶出,推测此可能为二者配伍后药效增强的原因。     

GC法测定不同品种莪术药材中3种成分的含量

目的建立莪术药材中β-榄香烯、=牛儿酮和莪术二酮的GC含量测定方法 ,并比较不同品种莪术药材中3种成分的含量。方法采用DB-225毛细管柱,FID检测器。结果β-榄香烯、=牛儿酮和莪术二酮的线性范围分别为：1.019-5.095mg.mL-1（r=1.0000）;1.0609-10.609mg.mL-1（r=0.9999）;2.218-4.436mg.mL-1（r=0.9999）。平均回收率分别为：β-榄香烯100.6%,RSD=1.95%（n=9）;=牛儿酮100.6%,RSD=1.85%（n=9）;莪术二酮99.6%,RSD=2.13%（n=9）。结论不同品种莪术药材挥发油中莪术二酮的含量存在显著性的差异。该法准确、可靠,可用于莪术药材的质量控制。     

促渗剂对莪术软膏中莪术醇、吉马酮透皮吸收的影响

目的:研究不同促渗剂对莪术软膏中莪术醇、吉马酮透皮吸收的影响。方法:采用Franz扩散池法,以离体大鼠皮肤为透皮屏障,以高效液相色谱法测定加入不同促渗剂(3%冰片、3%薄荷脑、3%冰片+3%薄荷脑)的莪术软膏中莪术醇、吉马酮的累积渗透量,同时测定稳态透皮速率以计算增渗倍数。色谱柱为Diamonsil C18,流动相为乙腈-1%磷酸溶液(梯度洗脱),柱温为25℃,流速为1.0 ml/min,检测波长为216 nm,进样量为20μl。结果:莪术醇、吉马酮检测质量浓度的线性范围分别为9.62~47.11μg/ml(r=0.999 1)、33.61~167.82μg/ml(r=0.999 5);精密度、稳定性试验的RSD均小于2.05%,回收率为99.42%。加入3%冰片、3%薄荷脑、3%冰片+3%薄荷脑后莪术醇、吉马酮10 h平均累积渗透量分别为221.21、209.92、269.44μg/cm2与506.74、480.85、615.67μg/cm2;莪术醇、吉马酮6 h增渗倍数分别为1.62、1.41、1.85与1.66、1.50、2.13。结论:3%冰片+3%薄荷脑对莪术醇和吉马酮促渗效果最佳;本试验为莪术软膏的深入研究提供了一定的理论基础。     

GC-MS测定莪术油聚氰基丙烯酸正丁酯毫微粒中4个成分的含量

目的:建立测定莪术油聚氰基丙烯酸正丁酯毫微粒(ZTO-PBCA-NP)中莪术油的主要成分β-榄香烯、莪术酮、莪术醇和莪术二酮含量的气相色谱-质谱方法。方法:采用HP-5MS毛细管色谱柱(30.0 m×250μm×0.25μm),进样温度250℃,不分流;程序升温:初始65℃恒温2 min,以5℃.min-1升至90℃恒温3 min,以20℃.min-1升至103℃恒温3 min,以8℃.min-1升至150℃恒温15 min,以20℃.min-1升至280℃。结果:β-榄香烯、莪术酮、莪术醇和莪术二酮进样浓度在4.00～40.00μg.mL-1范围内与峰面积呈良好线性关系(r=0.9979～0.9997);平均回收率(n=4)分别为98.3%(RSD=2.8%),99.4%(RSD=2.1%),95.5%(RSD=1.6%),101.2%(RSD=2.5%)。结论:该方法专属性强,准确度高,重复性好,可用于ZTO-PBCA-NP的质量控制。     

毛细管气相色谱法同时测定保妇康栓中冰片及3种倍半萜含量

目的建立GC-FID含量测定方法,同时测定保妇康栓中冰片、呋喃二烯、莪术醇和莪术二酮的含量。方法采用HP-5石英毛细管色谱柱(30 m×0.25 mm,0.25μm)程序升温,流速为2.5 mL.min-1,分流比为10∶1,进样量为1μL。结果冰片、呋喃二烯、莪术醇和莪术二酮质量浓度分别在28.0～224.0(r=0.999 8)、16.0～128.0(r=0.999 9)、2.8～22.4(r=0.999 8)、4.0～32.0 mg.L-1(r=0.999 9)内线性关系良好,平均回收率分别为103.7%、91.6%、102.5%、99.5%,RSD分别为4.7%、3.6%、3.9%、4.3%(n=9)。结论本方法可为保妇康栓的质量控制提供科学依据。     

黄芪莪术不同比例配伍后莪术4种挥发性成分的含量变化研究

目的： 探究黄芪莪术不同配伍比例中,莪术挥发油中抗肿瘤活性成分含量的变化。方法：水蒸气蒸馏法对挥发油进行提取,运用气相色谱法,测定单味莪术及黄芪莪术配伍比例为1∶1、2∶1、3∶1、5∶1、1∶2中β-榄香烯、莪术醇、吉马酮、新莪术二酮的含量。采用HP-5气相色谱柱,程序升温法,进样口温度为 250℃,FID检测器温度为280℃;内标物质是水杨酸甲酯。结果：β-榄香烯、莪术醇、吉马酮、新莪术二酮4种挥发油分别在0.003 0 ~ 0.192 0 mg·mL-1（r = 0.996 9）、0.023 3 ~ 2.979 0 mg·mL-1（r = 0.999 3）、0.005 9 ~ 0.376 0 mg·mL-1（r = 0.999 4）、0.017 5 ~ 1.118 0 mg·mL-1（r = 0.994 3）范围呈良好的线性关系,黄芪、莪术以2∶1的比例配伍时,各成分溶出量最高。结论：随着黄芪莪术配伍比例的不同,挥发油中抗肿瘤成分含量有所变化,以2∶1、3∶1的配伍比例为佳,为临床应用和药效学研究提供依据。     

采挖期内不同月份对广西桂莪术挥发油的影响

目的 考察采挖期内不同月份对桂莪术主要成分的影响.方法 利用挥发油提取器提取,比较不同采收月份桂莪术挥发油含量;运用HPLC法测定不同采收月份中吉马酮的含量,色谱柱为C18柱(4.60×250mm,5μm),流动相为乙腈-水(67∶33),检测波长210nm,流速为1.0mL·min-1;柱温为35℃.结果 HT6K 10月份采挖的桂莪术挥发油含量最高,11月份桂莪术吉马酮含量最高.结论 采挖期内不同月份桂莪术挥发油和吉马酮含量差异明显.     

高效液相色谱法测定莪术中吉马酮的含量

目的 :建立以高效液相色谱法测定莪术中吉马酮含量的方法。方法 :色谱柱为C18,流动相为乙腈 -水 (梯度洗脱 ) ,流速为1 .0ml/min ,检测波长为214nm。结果 :吉马酮检测浓度在0. 95～285μg/ml范围内线性关系良好 (r=0 .9999) ,平均回收率为97.89 % (RSD=2.52 % ,n=5)。结论 :本方法简便、可靠 ,可用于莪术药材的含量测定和质量控制。     

Alkaloids from Aspidosperma species from Bolivia

Two Bolivian Aspidosperma species were investigated. The seed and stem bark of Aspidosperma macrocarpon Mart. contain six known alkaloids: (-)-vincadifformine, ervinceine, kopsanone, kopsinine, kopsanol in the seed, and kopsanone, kopsinine, kopsanol, 18-epikopsanol in the stem bark. The stem bark of Aspidosperma pyrifolium Mart. contains eleven known alkaloids: (-)-vincadifformine, O-demethylpalosine, haplocine, N-formylaspidospermidine, vallesine, demethoxyaspidospermine, palosine, (-)-aspidospermine, aspidospermidine, akuammicine, tubotaiwine, beside the two new bases dehydroxyhaplocidine and 10-methoxyaspidospermidine.     

Emerging biopharmaceuticals from bioactive peptides derived from marine organisms

Biologically active natural products are spontaneous medicinal entrants, which encourage synthetic access for enhancing and supporting drug discovery and development. Marine bioactive peptides are considered as a rich source of natural products that may provide long‐term health, in addition to many prophylactic and curative medicinal drug treatments. The large literature concerning marine peptides has been collected, which shows high potential of nutraceutical and therapeutic efficacy encompassing wide spectra of bioactivities against a number of infection‐causing agents. Their antimicrobial, antimalarial, antitumor, antiviral, and cardioprotective actions have achieved the attention of the pharmaceutical industry toward new design of drug formulations, for treatment and prevention of several infections. However, the mechanism of action of many peptide molecules has been still untapped. So in this regard, this paper reviews several peptide compounds by which they interfere with human pathogenesis. This knowledge is one of the key tools to be understood especially for the biotransformation of biomolecules into targeted medicines. The fact that different diseases have the capability to fight at different sites inside the body can lead to a new wave of increasing the chances to produce targeted medicines.     

Decreased sensitivity of isolated hepatocytes from baby rats,from regenerating and from poisoned livers to phalloidin

Summary Isolated hepatocytes, prepared from 5 day old rats, from regenerating livers or from livers after poisoning with carbon tetrachloride, are less sensitive to phalloidin in vitro than hepatocytes from untreated adult controls. The time course of the reduced susceptibility to phalloidin was compared with the ability of hepatocytes to take up bile acids under various conditions. SDS-electrophoresis of cell lysates gave no evidence for decreased levels of actin in cells with reduced sensitivity to phalloidin. In contrast, there was a good relationship between the active uptake of bile acids and the sensitivity of hepatocytes to phalloidin. The decreased response of hepatocytes from baby rats, from regenerating livers or from poisoned livers to phalloidin is more probably related to differences in phalloidin uptake than to a reduced endowment with microfilamentous structures.This work is supported by the Deutsche Forschungsgemeinschaft     

Drug release from laminated polymeric films prepared from aqueous latexes

Laminated films comprised of a drug-containing reservoir layer and a drug-free, rate-controlling membrane were prepared from aqueous latexes and investigated as an alternative drug delivery system to polymeric films cast from organic solvents. The reservoir layer was prepared by casting and drying the latex [copolymer of poly(ethylacrylate-methylmethacrylate) esters - Eudragit NE 30D (NE 30D)] containing the dissolved drugs (chlorpheniramine maleate, propranolol HCl, or salicylic acid). Monolithic solutions (salicylic acid-NE 30D) or dispersions (chlorpheniramine maleate or propranolol HCl-NE 30D) were formed, depending on the solubility of the drug in the polymer matrix. Zero-order drug release was achieved by laminating a second, drug-free latex film onto the reservoir layer. The rate-controlling membrane was either attached to, or cast directly onto the reservoir. The release rate was independent of loading for the monolithic dispersions, but dependent on loading for the monolithic solution. Release rates were enhanced by the addition of a hydrophilic polymer, hydroxypropyl methylcellulose, to the rate-controlling membrane. An inverse relationship was observed between the release rate and membrane thickness. The rate-controlling membrane, cast from organic polymer solutions, had a denser structure, resulting in slower drug release when compared with latex-cast laminates.     

Composition of the essential oil from Thymus moesiacus from Macedonia

Composition of the essential oil of Thymus moesiacus Velen. from Macedonia was examined by GC and GC-MS methods. The main constituents of the oil were geraniol, linalool, geranyl acetate, and terpenyl acetate.