HPLC法测定麻杏抗感颗粒中盐酸麻黄碱和盐酸伪麻黄碱的含量

目的 建立麻杏抗感颗粒中盐酸麻黄碱和盐酸伪麻黄碱的含量测定方法。方法 采用高效液相色谱（HPLC）法,色谱柱：Wondasil C₁₈（4.6 mm×250 mm,5 μm）;流动相：乙腈-0.1%磷酸溶液（5：95）;流速：1 ml/min;检测波长：215 nm;柱温：30℃;进样量：10 μl。结果 盐酸麻黄碱、盐酸伪麻黄碱的质量浓度分别在4.231~42.31 μg/ml（r=0.999 7）、1.187~11.87 μg/ml（r=0.999 9）范围内与各自峰面积线性关系良好,平均加样回收率为分别为98.9%、98.1%;RSD分别为0.48%、0.64%。结论 该法准确度高、重复性好, 可用于麻杏抗感颗粒中盐酸麻黄碱和盐酸伪麻黄碱的含量测定。     

用HPLC法同时测定自制复方特比萘酚软膏中3个主药成分的含量

目的 建立同时测定自制复方特比萘酚软膏中3个主药成分含量的HPLC法。方法 色谱柱为ZORBAX SB-C₈柱（4.6 mm×250 mm,5 μm）,流动相为甲醇-0.1%磷酸溶液（70∶30）,柱温：30 ℃,流速：1.0 ml/min,检测波长：248 nm,进样量：10 μl。结果 盐酸特比萘芬在20.4～204.0 μg/ml（r =0.999 7）,莫匹罗星在40.4～404.0 μg/ml（r=0.9998）,糠酸莫米松在2.02～20.20 μg/ml（r=0.999 7）的浓度范围呈良好的线性关系,加样回收率分别为99.39%、99.21%、99.97%,RSD分别为0.82%、0.59%、0.81%（n=9）。结论 该方法的专属性、重复性良好,可用于自制复方特比萘酚软膏中的特比萘酚、莫匹罗星、糠酸莫米松的含量测定。     

双波长HPLC法测定止痒地霜中地塞米松和羟苯乙酯的含量

目的 建立双波长HPLC法同时测定止痒地霜中地塞米松磷酸钠和羟苯乙酯的含量。方法 采用RP-HPLC法,以Wondasil C₁₈（4.6 mm×250 mm,5 μm）为色谱柱,以三乙胺溶液-甲醇-乙腈（52：43：5）为流动相;检测波长为242 nm,流速为1.0 ml/min。结果 羟苯乙酯和地塞米松磷酸酯分别在21.42～64.26 μg/ml （r=1.0000）和20.84～62.53 μg/ml （r=0.9999）范围内有良好的线性关系,平均回收率分别为99.1%（RSD=0.41%）和99.0%（RSD=0.72%）。结论 该法简便、准确、重复性好,可用于止痒地霜的质量控制。     

HPLC法测定复方苯海拉明乳膏中盐酸苯海拉明的含量

目的 建立HPLC法测定复方苯海拉明乳膏中盐酸苯海拉明的含量。方法 色谱柱为ACE5C₁₈S/N-A66766柱（150 mm×4.6 mm,5 μm）;流动相为甲醇-水-三乙胺（70:30:0.67,用磷酸调pH为6.5）;检测波长设定230 nm;流速设定1.0 ml/min;乳膏经过提取净化后进样20 μl在室温下分析。结果 盐酸苯海拉明在39.52～197.6 μg/ml范围内线性关系良好（r=0.999 7）,平均回收率为100.5%（RSD=1.25%,n=9）,重复性结果显示RSD为0.78%（n=6）,所测得盐酸苯海拉明乳膏含量结果为标示量的101.3%、99.83%、99.62%。结论 本方法准确、灵敏、专属性强、重现性好,对复方苯海拉明乳膏质量控制标准的提高具有参考意义。     

高效液相色谱法测定不同产地假蒟中的α-细辛脑含量

目的 采用高效液相色谱（HPLC）法测定不同产地假蒟中α-细辛脑的含量。方法 色谱柱为Lichrospher C₁₈柱（150 mm×4.6 mm,5 μm）,流动相为乙腈-0.05%磷酸溶液（47：53）,流速为1.0 ml/min,检测波长313 nm,柱温30℃。结果 α-细辛脑在0.0970~1.934 μg范围内与峰面积有良好线性关系（r=0.999 8）,平均回收率为99.94%（RSD=1.13%）,样品在24 h内稳定,且该方法重复性较好。结论 本方法简便准确,可用于假蒟药材中α-细辛脑的含量测定,以控制其质量;我国不同产地的假蒟中α-细辛脑含量有明显差异,其中以广西产假蒟含量最高。     

用HPLC法测定人凝血酶制品中甘氨酸的含量

目的 建立一种测定人凝血酶制品中甘氨酸含量的HPLC方法。方法 以2、4-二硝基氟苯（DNFB）为柱前衍生剂,采用ODS-C₁₈色谱柱,流动相为50%乙腈溶液-0.05 mol/L醋酸钠缓冲液（35︰65）,流速1.0 ml/min,检测波长360 nm。结果 甘氨酸的线性范围为0.006~0.030 mg/ml（r=0.999 6）,平均回收率为100.4%,RSD为0.44%（n=9）。结论 该方法简便、准确、专属性好,可用于人凝血酶制品中甘氨酸的含量测定。     

高效液相法测定陈皮药渣中橙皮苷含量

摘 要 目的:通过对陈皮药材及药渣中橙皮苷含量进行比较分析,为陈皮药渣的二次开发提供依据。方法: 色谱柱:Eclipse XDB- C₁₈(280 mm×4.6 mm, 5 μm)流动相：甲醇∶水∶冰醋酸（30∶66∶4）;流速：1.0 ml·min^-1;检测波长：283 nm。结果:橙皮苷与其它色谱峰分离良好。橙皮苷的线性范围在0.42～4.20 μg,r=0.999 7。陈皮药材的平均加样回收率为98.5%,RSD=2.12%(n=6);陈皮药渣的平均加样回收率为98.1%,RSD=2.35%(n=6)。结论:陈皮药渣中橙皮苷的提取量为陈皮药材中橙皮苷的提取量52%,表明陈皮药渣具有二次开发利用的价值。     

健脾补肾颗粒的质量标准研究

目的 建立健脾补肾颗粒的质量标准。方法 采用薄层色谱法（TLC）鉴别制剂中黄芪、丹参、党参、陈皮和白芍五味药材。用高效液相色谱法（HPLC）测定白芍中芍药苷的含量：色谱柱：Agilent Eclipse Plus C₁₈柱（4.6 mm×250 mm,5 μm）;流动相：乙腈-0.1%磷酸水溶液梯度洗脱;流速：1.0 ml/min;柱温：25℃;检测波长：230 nm。结果 5种药材的TLC图谱斑点清晰,无阴性对照干扰;芍药苷在8.676~277.632 μg/ml范围内线性关系良好,（r=0.999 9）。结论 该法操作简单、重复性好,能够有效控制健脾补肾颗粒的质量。     

高效液相色谱法测定新保肾片中芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的含量

目的 建立新保肾片中芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的含量测定方法,为生产质量提供保障。方法 采用高效液相色谱法测定,色谱柱为Lichrospher-C₁₈柱(250 mm ×4.6 mm,5 μm),流动相为甲醇:0.1%磷酸溶液(7030),流速为1.0 ml/min,柱温为35 ℃,检测波长为254 nm。结果 芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚分别在2.30~18.4 μg/ml(r=1.0)、2.930~23.44 μg/ml(r=1.0)、5.00~40.0 μg/ml(r=1.0)、14.870~118.96 μg/ml (r=0.999 8)、7.410~59.28 μg/ml(r=0.999 9)范围内有良好的线性关系,平均回收率分别为100.16%、102.91%、99.76%、100.32%、100.44%,RSD分别为1.58%、1.27%、1.67%、1.33%、1.03%(n=9)。结论 该方法准确易行,便于质量控制。     

用HPLC法测定百蕊草中3个黄酮苷的含量

目的 建立HPLC法同时测定百蕊草中3个黄酮苷类化合物的含量。方法 色谱柱为DIKMA C₁₈柱（250 mm×4.6 mm,5 μm）,流动相为乙腈-水（21∶79,V/V）,用冰醋酸调节pH至4.61,流速：1.0 ml/min,柱温：25℃,检测波长：346 nm。结果3个黄酮苷化合物山奈酚-3-O-L-吡喃鼠李糖基（1→2）-β-D-吡喃葡萄糖苷（百蕊草素Ⅰ）、山奈酚-3-O-β-D-吡喃葡萄糖苷（紫云英苷）、山奈酚-3-O-L-吡喃鼠李糖基（1→2）-[6-O-乙酰基]-β-D-吡喃葡萄糖苷（6''-乙酰氧基百蕊草素Ⅰ）的进样浓度分别在125~200、2.5~40、5.0~80 μg/ml范围内线性关系良好（r=0.999 9）,平均加样回收率分别为101.63%、99.82%和102.02%,RSD分别为1.72%、2.34%和1.94%（n=6）。结论 该方法准确,稳定性、重现性好,可作为百蕊草药材及制剂的质控方法。     

Synthesis and evaluation of 2,6-piperidinedione derivatives as potentially novel compounds with analgesic and other CNS activities

New 2,6-piperidinediones 2_a–g and 4_a–d were prepared by initial condensation of aromatic aldehydes or cycloalkanones with cyanoacetamide to give α-cyanocinnamides l_a–g or cycloalkylidenes 3_a,b which underwent Michae1 addition with ethyl cyanoacetate or diethylmalonate. Compounds 4_a–d were alkylated by various alkyl halides to produce the N-alkylated 2,6-piperidinedione derivatives 5_a–m. Some new selected compounds 2_a–c,f, 4_a–d & 5_e,h,j were pharmacologically evaluated for potential anticonvulsant, sedative and analgesic activities. These compounds exhibited significant anticonvulsant and analgesic effects after a single I.P. administration 100 mg/kg b.wt. . On the other hand all the investigated compounds induced hypnotic activity and prolonged the phenobarbital sodium- induced sleep as compared with the control group and the most potent compound was found to be 2_f.     

鼻渊净胶囊的HPLC指纹图谱研究

目的 建立鼻渊净胶囊的高效液相色谱(HPLC)指纹图谱.方法 采用Agilent SB-C18(4.6 mm×250 mm,5μm)色谱柱,乙腈-水为流动相、以1.0 ml/min流速行梯度洗脱,检测波长210 nm,柱温30℃,洗脱时间为80 min.采用中药色谱指纹图谱相似度评价系统(2004A版)对检测出色谱进行...     

EFFECT OF POLICOSANOL SUCCESSIVE DOSE INCREASES ON PLATELET AGGREGATION IN HEALTHY VOLUNTEERS

Policosanol is a cholesterol-lowering drug with hypocholesterolemic effects demonstrated in experimental models, healthy volunteers and type II hypercholesterolemic patients. In addition, antiplatelet effects of policosanol have been shown in experimental models and healthy volunteers. The effect of successively increasing doses of policosanol on platelet aggregation was investigated in a randomized, placebo-controlled, double-blind study conducted in 37 healthy volunteers. The volunteers were on a placebo-baseline period (two tablets per day) for 7 days and thereafter they received randomly, under double-blind conditions, placebo or policosanol (10mgday⁻¹) for 7 days. After this period dosage was doubled to 20mgday⁻¹for the next 7 days and then again doubled to 40mgday⁻¹, while the control group received placebo tablets all the time. Platelet aggregation as well as coagulation time was measured at baseline and after each dosing step. Results showed that antiplatelet effects of policosanol were successfully enhanced throughout the study, thus suggesting a dose-dependent relationship. No significant effect was reached during the first dosing period, but significant reductions of epinephrine and ADP-induced platelet aggregation were observed after the second one. Finally, a significant inhibition of platelet aggregation induced by all the agonists was observed at the last dosing step. Coagulation time remained unchanged during the trial.     

NEURAMIDE STIMULATES ADRENOCORTICOTROPIN BUT NOT PROLACTIN RELEASE FROM RAT PITUITARY

Neuramide (NMD), a substance found in crude preparations of porcine stomach extract, is a viral inhibitor that also has putative immunostimulatory effects. The effects of NMD on stress-hormone (ACTH and prolactin—PRL) release were assessed inin vivoandin vitrostudies. In the former, blood levels of corticosterone and PRL were measured in NMD-treated male rats.In vitroexperiments were performed to evaluate the effects of NMD and three of its fractions (obtained with high performance liquid chromatography) on ACTH and PRL release from perfused rat pituitary slices. NMD increased plasma corticosterone levelsin vivoand produced dose-dependent increases inin vitropituitary release of ACTH. No effects on PRL secretion were observedin vivoorin vitro. The stimulatory effects on ACTH release were caused by the NMD fraction with a molecular weight of >5000<10000Da.     

Investigation of the prevalence of tetQ, tetX and tetX1 genes in Bacteroides strains with elevated tigecycline minimum inhibitory concentrations

In this study, the antibiotic susceptibilities to tigecycline and tetracycline of 35 selected Bacteroides fragilis group strains were determined by Etest, and the presence of tetQ, tetX, tetX1 and ermF genes was investigated by polymerase chain reaction (PCR). tetQ was detected in all 12 B. fragilis group isolates (100%) exhibiting elevated tigecycline minimum inhibitory concentrations (MICs) (≥8 μg/mL) as well as the 8 strains (100%) with a tigecycline MIC of 4 μg/mL, whilst tetX and tetX1 were present in 15% and 75% of these strains, respectively. All of these strains were fully resistant to tetracycline (MIC ≥ 16 μg/mL). On the other hand, amongst the group of strains with tigecycline MICs < 4 μg/mL (15 isolates), tetQ, tetX and tetX1 were found less frequently (73.3%, 13.3% and 46.7%, respectively). All but two strains harbouring the tetQ gene in this group were non-susceptible to tetracycline, with a MIC > 4 μg/mL. These data suggest that in most cases tigecycline overcomes the tetracycline resistance mechanisms frequently observed in Bacteroides strains. However, the presence of tetX and tetX1 genes in some of the strains exhibiting elevated MICs for tigecycline draws attention to the possible development and spread of resistance to this antibiotic agent amongst Bacteroides strains. The common occurrence of ermF, tetX, tetX1 and tetQ genes together predicted the presence of the CTnDOT-like Bacteroides conjugative transposon in this collection of Bacteroides strains.     

INDIRECT PARASYMPATHOMIMETIC ACTIVITY OF THE CLASS III ANTIARRHYTHMIC SUBSTANCE / -SOTALOLIN VITRO: REVERSIBLE INHIBITION OF CHOLINESTERASE ISOENZYMES FROM BLOOD AND THE HUMAN CENTRAL NERVOUS SYSTEM

Inhibitory effects of the class III antiarrhythmic compound / -sotalol on acetylcholinesterase (AChE; EC 3.1.1.7) isoenzymes of both erythrocytes and the human caudate nucleus and on serum cholinesterase (ChE; EC 3.1.1.8) were studiedin vitrousing a spectrophotometric kinetic assay with acetylthiocholine (ASCh) as substrate. Sotalol concentrations in the assays varied from 0.32 to 3.2m . All isoenzymes studied were inhibited by / -sotalol in a reversible and concentration-dependent manner. Double reciprocal plots of the reaction velocity against varying ASCh concentrations revealed that / -sotalol reduced substrate affinity (apparent Michaelis constant, KM, increased) of serum ChE, but did not change the enzyme's maximal rate of ASCh hydrolysis (V_max). Thus, / -sotalol inhibition of serum ChE was of the competitive type (rate constant for reversible competitive inhibition: K_i=0.51m ). In contrast, / sotalol reduced the maximal reaction velocity of the AChE isoenzyme from the central nervous system (caudate nucleus), but had no influence on substrate affinity of the enzyme (K_Mwith ASCh unchanged) indicating purely non-competitive inhibition kinetics (rate constant of reversible non-competitive inhibition: K_i′=0.44m ). / -sotalol inhibition of erythrocyte AChE was of mixed competitive/non-competitive type (K_i=0.31m , K_i′=0.49m ). Non-competitive / -sotalol inhibition of caudate nucleus AChE and the non-competitive component of erythrocyte AChE inhibition cannot be overcome by increased concentrations of the cholinergic transmitter acetylcholine (ACh). Peak / -sotalol plasma levels as described in the literature for both humans (15μ ) and experimental animals (dogs: 18μ ; rats: 260μ ) as well as maximal myocardial concentrations of the substance (dogs: 46μ ; rats: 478μ ) are in the range of about 2% to 100% of the sotalol inhibition rate constants determined in the present paper for cholinesterase isoenzymesin vitro. Thus, / -sotalol inhibition of ACh hydrolysisin vivomay contribute to both the well known antiarrhythmic potential and proarrhythmic side effects of the compound.     

喙果黑面神化学成分研究

目的研究大戟科植物喙果黑面神(Breynia rostrata Merr.)的化学成分。方法利用硅胶、凝胶等色谱技术分离纯化化学成分,根据化合物的理化性质和光谱数据进行结构鉴定。结果从喙果黑面神的正丁醇萃取部分分离得到4个化合物,分别鉴定为6-O-甲基丙酰基-α-D-吡喃葡糖(6-O-methylpropanoyl-α-D-glucopyranose,1);4″-苯酚基-6-O-甲基丙酰基-β-D-吡喃葡糖苷(4″-phenolic-6-O-methylpropanoyl-β-D-glucopyranoside,2);1-O-没食子酰基-β-D-吡喃葡糖苷(1-O-galloyl-β-D-glucopyranoside,3);熊果苷(arbutin,4)。结论化合物1和2为新化合物,3和4均为首次从该种植物分离得到。     

EFFECTS OF 2-GUANIDINE-4-METHYLQUINAZOLINE ON GASTRIC ACID SECRETION IN RATS

In this study 2-guanidine-4-methylquinazoline (2-GMQ) appeared to decrease basal and stimulated gastric acid secretion, while structurally related compounds as dimethyl- biguanide, cyanoguanidine and 2-cyanoamino-4-methylpyrymidine did not. Thus, there is an antisecretory effect when the biguanide group is associated with a lipophilic structure. The antisecretive effects exerted by 2-GMQ are associated with anti H₂-histamine activity.The anti H₂-histamine nature of the effects of 2-GMQ was confirmed by the capacity of this compound of depressing the chronotropic activity of the isolated guinea pig auricle increased by histamine, as well as relaxant activity in rat uterus contracted by histamine, since both preparations are rich in H₂-histamine receptors.     

栝楼不同药用部位质量控制的研究进展

瓜蒌子、瓜蒌皮、瓜蒌、天花粉来源于栝楼的不同药用部位,4味药材均为常用的大宗药材,现行版《中国药典》对其制定的质量标准过于简单,无法科学合理地控制其质量。本文对瓜蒌子、瓜蒌皮、瓜蒌、天花粉安全性和有效组分的研究进行综述,明确了相关研究存在的问题并针对问题提出建议,为科学全面的药材及饮片标准的制定提供参考依据。     

AMELIORIATION OF CHEMICALLY-INDUCED HEPATOCYTE INJURY BY CYCLOSPORINE A

Cyclosporine A, beside its current applications, possesses potential hepatoprotective effects. This study was directed to investigate the effect of Cyclosporine A pretreatment on hepatic injury due to carbon tetrachloride (CCl₄) and -galactosamine. Rats were injected by two successive doses of Cyclosporine A (5mgkg⁻¹day⁻¹). Six hours after the second dose, 1mlkg⁻¹of CCl₄was administered i.p. Effects associated with Cyclosporine A pretreatment were examined by using isolated hepatocytes and hepatocytes that were immobilized and continuously perfused. -Galactosamine (5m ) was added directly to the perfusion medium. After isolation, hepatocytes were examined histologically by light and electron microscopy, immobilized and perfused for further metabolic functional activity evaluation. Cyclosporine A pretreatmentin vivoproduced hepatoameliorative effects of various degrees which were statistically significant as manifested by: (1) an increased trypan blue exclusion after CCl₄; (2) an improved ureagenesis after CCl₄; (3) a reduction in the lipid droplets accumulation in the cytoplasm produced by CCl₄administration; (4) well preserved cytoplasmic organelles as mitochondria, endoplasmic reticulum ER, nuclear chromatin structures that were altered by CCl₄; and (5) an increased hepatocytes survival in the agarose gel matrix, reduction of LD leakage and improvement of ureagenesis after -galactosamine addition to the perfusion medium. The beneficial effect of Cyclosporine A pretreatment in modifying hepatotoxicity of chemical insults merits further studies.