HPLC测定山楂中金丝桃苷的含量

目的:建立HPLC法测定山楂中金丝桃苷含量的方法.方法:色谱柱SinoChrom ODS-BP(4.6mm×250mm,5μm);流动相:乙腈(A)-0.05％磷酸水(B)梯度洗脱(0～55min,11％～20％A;55～60min,20％～40％A;60～80min,40％～50％A);流速1.0mL·min-1;检测波长355nm;柱温35℃.结果:金丝桃苷在0.10～2.00μg范围内线性关系良好(r=1),平均回收率为98.61％,RSD为2.08％;山楂中金丝桃苷的平均含量为17.73mg·.结论:本方法操作简便,重现性好,结果准确,可用于山楂中金丝桃苷的含量测定.     

HPLC法测定药材贯叶金丝桃中金丝桃苷和槲皮素的含量

目的建立测定药材贯叶金丝桃中槲皮素和金丝桃苷含量的方法。方法采用高效液相色谱法(HPLC)。色谱柱:Hypersil CN(150mm×4.6mm,5μm);流动相:甲醇-4mL·L-1磷酸(30/70),流速1.0mL·min-1;检测波长(241,360nm);柱温30℃;进样量20μL。结果槲皮素和金丝桃苷浓度分别在0.02~10和0.03~8μg·mL-1质量范围内与峰面积积分分值呈良好线性关系。加样回收率分别为98.0%和98.1%。结论该方法专属性强,灵敏度高,重复性好,可作为该药材测定槲皮素和金丝桃苷质量控制的方法。     

HPLC测定菟丝子中金丝桃苷与槲皮苷的含量

目的用HPLC测定菟丝子中金丝桃苷与槲皮苷的含量。方法采用ShimadzuC18柱(150mm×4.6mm,5μm),流动相为甲醇-0.2%H3PO4水溶液(45∶55),流速1.0ml·min-1,检测波长350nm,柱温为室温,用外标法定量,测定菟丝子中金丝桃苷与槲皮苷的含量。结果金丝桃苷的线性范围0.50～2.50μg(r=0.9998),回收率95.90%,RSD=0.93%;槲皮苷的线性范围0.40～2.00μg(r=0.9996),回收率99.19%,RSD=2.39%。结论所建方法简便,快速,线性关系良好。     

HPLC法同时测定贯叶金丝桃中芦丁、金丝桃苷和槲皮素的含量

目的建立贯叶金丝桃原药中芦丁、金丝桃苷和槲皮素的含量测定方法。方法样品经丙酮超声波辅助提取,采用Diamonsil~C_(18)柱(250mm×4.6mm,5μm)分离测定;以A相乙腈-甲醇-甲酸(89.8∶10∶0.2),B相水-甲醇-甲酸(79.8∶20∶0.2)为流动相梯度洗脱;检测波长为270nm;流速为1.0mL·min~(-1)。结果芦丁的进样量在0.454~4.540μg范围内(r=0.999 7),金丝桃苷的进样量在0.480~4.800μg范围内(r=0.999 2),槲皮素的进样量在0.794~7.940μg范围内(r=0.999 5),都与峰面积线性关系良好。加样回收率分别为99.01%,96.04%和95.97%(n=6)。结论该方法快捷、简便,结果准确、可靠,可作为贯叶金丝桃原药中有效成分的质量控制方法。     

HPLC测定金荞麦中的金丝桃苷

目的 测定金荞麦中金丝桃苷的含量.方法 采用HPLC法,色谱柱为Shimadzu C18(150 mm ×4.6 mm,5 μm),流动相为甲醇-0.2%H3PO4溶液(45:55),流速为1.0 ml·min-1,检测波长为350 nm,柱温为室温,用标准曲线法定量,测定金荞麦中金丝桃苷的含量.结果 金丝桃苷0.5～2.5 μg与峰面积的线性关系良好(r=0.9998),回收率为95.01%,RSD=2.94%.结论 所建方法简便、快速,适用于金荞麦中金丝桃苷的测定.     

HPLC 法测定贯叶金丝桃中芦丁和金丝桃苷的含量

目的：建立贯叶金丝桃中芦丁与金丝桃苷的含量测定方法。方法：采用高效液相色谱仪,使用Diamonsil C18柱（250mm×4.6 mm,5μm）,流动相为甲醇-乙腈-四氢呋喃-0.4%醋酸（1∶1∶18∶80）,流速为0.7 ml·min-1,检测波长为358 nm,柱温为30℃。结果：芦丁在0.206～1.236μg范围内有良好的线性关系,r=0.999 9。金丝桃苷在0.144～0.864μg范围内有良好的线性关系,r=0.999 8;芦丁的平均加样回收率为98.57%,RSD为0.94%,金丝桃苷的平均加样回收率为98.57%,RSD为0.94%。结论：该方法简便快捷,准确度高。     

RP-HPLC法测定照山白中金丝桃苷的含量

目的:建立照山白药材中金丝桃苷的含量测定方法。方法:样品用90％的乙醇回流提取,提取液滤过,以RP-HPLC法测定,用DiamonsilTMC18色谱柱(250 mm×4.6 mm,5μm),以甲醇-5％磷酸-三乙胺(45:55:0.36)为流动相,流速为1.0mL·min-1,检测波长为360nm。结果:金丝桃苷的保留时间约为15 min,且与其它峰的分离度大于1.5。金丝桃苷的线性范围为0.12-0.28μg(r=0.9999),最低检测限为2.9 ng,定量限为0.029μg,平均回收率和RSD分别为99.8％和0.90％。结论:该方法简便快速,结果准确可靠,可为照山白药材的质量评价提供有效手段。     

RP-HPLC法测定不同产地不同部位贯叶金丝桃中金丝桃苷的含量

目的：建立测定贯叶金丝桃中金丝桃苷含量的方法,并测定不同产地不同部位贯叶金丝桃中金丝桃苷的含量。方法：采用反相高效液相色谱法。色谱柱为Boston Breeze-C18（250mm×4.6mm,5μm）,流动相为甲醇-0.1%磷酸水溶液（40∶60,V/V）,检测波长为360nm,流速为1.0mL·min-1。结果：金丝桃苷进样浓度在0.14～2.80μg·mL-1范围内与峰面积积分值呈良好的线性关系（r=0.9994）,平均加样回收率为95.97%,RSD=1.16%（n=6）。四川产地贯叶金丝桃花、叶中的金丝桃苷含量最高。结论：本方法简便、准确、重复性好,可用于贯叶金丝桃的质量控制。     

不同采收期及药用部位的长柱金丝桃中有效成分的含量变化

目的 考察长柱金丝桃药用部位、采收期对金丝桃苷和金丝桃素的含量变化.方法 采用HPLC法,色谱柱为Agilent Zorbax Extend-C18 (250 mm×4.6 mm,5 μm),金丝桃苷的流动相为乙腈-0.4％磷酸梯度洗脱,柱温为室温,检测波长360 nm,流速1.0mL·min-1;金丝桃素流动相为甲醇-0.1 mol·L-1磷酸二氢钠(90∶10),柱温为室温,流速为1.0 mL·min-1,检测波长590nm.结果 长柱金丝桃花中金丝桃苷及金丝桃素的含量最高;长柱金丝桃在5月中旬其有效成分含量达到最高,后又逐渐降低.结论 长柱金丝桃中金丝桃苷和金丝桃素的含量随着采收时间的不同而不同,而且不同器官中含量差异显著.     

HPLC法测定连蒲胶囊中金丝桃苷的含量

目的:建立测定连蒲胶囊中金丝桃苷含量的高效液相色谱法。方法:采用HPLC法,色谱柱为Agilent ZORBAX SB-C18(4.6 mm×250 mm,5μm);流动相为乙睛-0.5%磷酸溶液(16∶84);检测波长360 nm;流速1.0 mL.min-1。结果:金丝桃苷的进样量在0.026～1.037μg范围内线性关系良好(r=1.000 0),平均回收率为102.2%,RSD=0.4%(n=6)。结论:该方法灵敏、准确,重现性好,能有效地控制连蒲胶囊的内在质量。     

黑龙江省两种金丝桃属植物理化鉴别特征

目的：为了探讨黑龙江省两种金丝桃属植物长柱金丝桃(Hypericum ascyron L．)、乌腺金丝桃(H．attenuatum Choisy．)理化鉴别特征。方法：分别采用黄酮、皂苷、鞣质及金丝桃素的鉴别试验。结果：黄酮定性反应均为阳性；皂苷定性反应表明均含三萜皂苷；鞣质的定性反应表明它们所含鞣质为缩合鞣质；金丝桃素的定性反应表明乌腺金丝桃含金丝桃素。结论：二者理化鉴别特征有一定差别．能通过化学鉴别方法予以鉴别。     

Deriving health utility values from a randomized,double-blind,placebo-controlled trial of siltuximab in subjects with multicentric Castleman’s disease

Purpose: To estimate health utility values, explore predictors of utility values, and estimate the quality-adjusted life years (Q.A.L.Y.s) gained by treatment in multicentric Castleman’s disease (M.C.D.). Methods: The SF-36 was administered to 79 patients enrolled in a randomized, double-blind, placebo-controlled, multi-national study to determine the safety and efficacy of siltuximab plus best supportive care (B.S.C.) compared with B.S.C., in subjects with symptomatic M.C.D. Utility (SF-6D) scores were derived from the SF-36. Sensitivity analyses using utilities obtained by mapping the SF-36 to the EQ-5D were also conducted. Repeated measures, mixed effects models were conducted to estimate effects of treatment, responder status and?≥?Grade 3 adverse events (A.E.s) on changes in utility values over time, controlling for baseline utility value. Additionally, differential Q.A.L.Y. gain was assessed in the trial using multiple regression. Results: Patients on siltuximab and those who experienced a complete or partial response had higher mean utility values over time than those on placebo or those with stable disease. After an initial response to treatment, the mean utility remained relatively stable for patients on siltuximab and those who experienced a complete or partial response during the period when most patients were on study. A significantly different Q.A.L.Y. gain was found for patients on siltuximab (versus placebo) as calculated by SF-6D (0.070 Q.A.L.Y.s, p?<?.05) scores at 6 months (EQ-5D 0.096 Q.A.L.Y.s, p?<?0.05). Conclusions: Siltuximab demonstrated improved, durable health utility gains in this rare disease over B.S.C. The main SF-6D results were supported by EQ-5D sensitivity analysis. These findings are limited by the small study sample size and substantial missing data caused predominantly by crossover. A longitudinal, multisite international observational study capturing clinical, safety and health-related quality of life (H.R.Q.L.) endpoints are needed to confirm these findings.     

Behavioral effects of acrylamide in the mouse

The behavioral toxicity of acrylamide was characterized in the mouse by comparing standard measures of toxicity such as body weight loss and mortality with measures of hindlimb grip strength, locomotor activity, and appetitive behaviors including episodic milk-licking. In the latter test, the mouse received 15-min access daily to a highly palatable, nonessential food substance (10% sweetened milk) that was not available in the maintenance diet. Two strains of mice, CD-1 and $\text{C57BL}\text{6J}$, were injected ip five times weekly with either saline, 20, 60, or 100 mg/kg of acrylamide. Subchronic, but not acute, administration of 100 mg/kg produced weight loss, a severe neuropathy within 3 days, and 100% mortality within 2 weeks. Mice receiving 60 mg/kg subchronically had only a slight loss of body weight but developed a neuropathy within 3 weeks of dosing at which time there was a 50% mortality. Preceding these signs of toxicity, there was a highly significant increase in episodic milk-licking; this increase was significant in both strains of mice by Day 2 and remained elevated throughout the dosing period. The 20 mg/kg dose of acrylamide decreased hindlimb grip strength after 5 weeks of dosing but did not affect milk-licking or body weight even after 7 weeks of dosing. The new use of this test of appetitive behavior has documented a robust effect of acrylamide which preceded other signs of toxicity. The appearance of the various toxic signs was better predicted by the magnitude of the daily dose than the cumulative dose. This study also demonstrated the feasibility of using the mouse in behavioral toxicology.     

HPLC法测定人参、西洋参和三七不同部位中人参皂苷的含量

目的:为了探讨人参、西洋参和三七中人参皂苷的资源含量,以确保人参、西洋参和三七中人参皂苷资源充分被利用,为开发以人参皂苷为主的创新药物提供科学数据。方法:采用高效液相色谱法对人参、西洋参和三七不同部位中人参皂苷的含量进行测定。色谱条件为:Agilent 1100 Series 高效液相色谱仪;色谱柱为德国 Nucleosil-C_(18)(4.6 mm×150 mm,5μm);流动相为水-乙腈梯度洗脱,流速1.5 mL·min~(-1);A为水,B为乙腈;梯度洗脱程序为:0～16 min,56%B;16～20 min,56%→100%B;20～38 min,100%B;38～45 min,100%→56%B;45～60 min,56%B;60～70 min,56%B。所有组分均70 min 内出完。检测波长203 nm,柱温35℃,灵敏度为0.02AUFS。线性关系考察r=0.9994;精密度试验 RSD=0.26%,平均回收率为99.88%,重现性试验 RSD=2.0%,分离度为R=3.042。结果:人参须根含有较高的人参皂苷 Rb_1(1.082%),人参茎叶则含有较高的人参皂苷 Rc(1.002%)、Re(3.430%)和 Rg_1(1.303%);西洋参根含有较高的人参皂苷 Rb_1(2.213%)和 Re(0.9188%),西洋参芦头中含有较高的人参皂苷 Rb_1(2.840%)和Re(1.224%);三七根含有较高的人参皂苷 Rb_1(2.163%)和 Rg_1(2.633%),三七芦头中含有较高的人参皂苷 Rb_1(4.376%)和 Rg_1(4.145%)。结论:高效液相色谱法分离、分析人参皂苷效果好、准确、迅速、简便,也可作为评价人参属植物质量的有效分析方法。建议对人参、西洋参和三七中含量较高的人参皂苷进行提取分离,直接用于创新药物的开发。     

四川翠雀属植物的一个新种

目的调查翠雀属植物,拓展新药源。方法野外调查。结果对采自四川省彭州市天台山的翠雀属Delphinium L.标本与其近缘种进行对比鉴别,认定它是一个新种。结论天台山翠雀花Delphinium tiantaishanenseW.J.Zhang et G.H.Chen,sp.nov.为一个新种。     

Inhibition of dopamine D-1 and D-2 binding sites in neuronal tissue by ascorbate

Ascorbic acid in concentrations that are usually included in the incubation mixture for studies of dopamine receptor binding sites inhibits the binding of radiolabelied dopamine to D-1 and D-2 sites.     

The prevention by (+)-Cyanidanol-3 of hepatitis-induced changes in the disposition of imipramine in the rat

The administration of (+)-Cyanidanol-3 [+)-catechin) to the rat using a subchronic dosing regime based on that currently used in the therapy of acute viral hepatitis in man, largely prevented the changes in the disposition of a single dose of [14C]imipramine hydrochloride induced by the hepatotoxin, D-(+)-galactosamine hydrochloride in rats. Complete return to normal pharmacokinetics was not attained due to interaction between (+)-Cyanidanol-3 and imipramine. Biliary excretion of imipramine metabolites was 79.3% of the dose in control rats. This was reduced to 69.3 and 39.8% by the separate administration of (+)-catechin and galactosamine respectively. Concurrent administration of (+)-Cyanidanol-3 and galactosamine resulted in 64.8% of the imipramine dose appearing in bile. These results were reflected in changes in faecal and renal excretion of imipramine metabolites in surgically unmodified rats in which galactosamine injection caused an elevation of urinary excretion from 31.0 to 69.8% of the imipramine dose. Concurrent Cyanidanol administration reduced the effect of galactosamine so that only 46.9% was excreted in urine. These changes were due to decreased biliary excretion and increased renal excretion of the glucuronide conjugates of 2-hydroxyimipramine, 2-hydroxydesmethylimipramine and 10-hydroxyimipramine. None of the treatments used impaired the overall ability of the rat to metabolize imipramine, although the plasma clearance of imipramine was reduced by 42% as a result of galactosamine administration and by 21% during treatment with (+)-catechin alone or combined catechin and galactosamine treatment.     

四川乌头属一新种和一新变种

目的 拓展新药源.方法 野外调查和采集.结果 对采自四川省会理县龙帚山的乌头属标本与其近缘种进行对比鉴别,认定1新种1新变种.结论 龙帚山乌头Aconitum longzhoushanense W.J.Zhang et G.H.Chen,sp.nov.为一个新种;长柄铁棒锤Aconitum flavum Hand.-Mazz.vat.longipetiolatum W.J.Zhang et G.H.Chen,var.nov.为一个新变种.     

消化性溃疡HP阴性和阳性状态下相关病因及胃粘膜组织学变化的研究

探讨消化性溃疡(PU)患者HP(-)及(+)状态下相关病因和胃粘膜组织病变。方法:139例内镜确诊的PU患者,胃溃疡48例,十二指肠溃疡79例,复合性溃疡12例。胃镜下取胃窦组织4块,分别作组织病理学检查和快速尿素酶检测。结果:122例(87.8％)HP(+),17例(12.2％)HP(-)。HP(+)PU HP感染仍为首要病因之一,因镜下粘膜病损多发生于胃角、小弯及球部,HP(-)PU病因则多达两个以上,内镜下病变亦较HP(+)者更为多样化。本组HP(-)PU病因依次:眼用NSAID(35.3％);伴随其他疾病(29.5％);曾服抗生素或H-2受体阻滞剂(29.4％);应激因素(5.8％)等。无论HP(-)或(+),PU患者病理组织学所表现的固有膜内淋巴细胞、单核细胞等慢性炎细胞浸润现象且无显著性差异。但胃窦粘膜的急性炎性反应Hp(+)者较HP(-)者有显著性差异(P<0.001)。结论:虽然HP(-)和PU(+)共同的发病机理仍为胃粘膜“保护性屏障”与“侵袭性”腔内因子之间的平衡失调,但两者在发病过程中的致病因子及组织形态学表现亦有差异。由此提示,对PU治疗的关键应在于针对不同病因选择相应的治疗方案。     

贵州产淫羊藿的质量研究

用ＲＰ－ＨＰＬＣ法，对产于贵州淫羊藿属植物９种２变种的６种主要黄酮类成分分析，确定贵州产的箭叶淫羊藿类群质量最好。另外除药典种类外，粗毛淫羊藿、黔北淫羊藿、不城淫羊藿等可药和，而分布较物黔岭淫羊藿不宜药用。我们建立的高效液相分析方法，可作为淫羊藿属植物的鉴定可靠手段。