反相高效液相色谱法测定复方磺胺嘧啶滴鼻液中磺胺嘧啶和盐酸麻黄碱含量

目的建立了一种反相高效液相色谱-紫外检测法用于复方磺胺嘧啶滴鼻液中磺胺嘧啶和盐酸麻黄碱的含量测定。方法色谱柱为Zorbax Bonus RP C18(150 mm×4.6 mm,5μm),流动相为0.050 mol.L-1磷酸二氢钾溶液(含0.5%三乙胺,用磷酸调节pH值至2.3)-甲醇(80∶20),盐酸麻黄碱的检测波长为216 nm,磺胺嘧啶为265 nm。结果磺胺嘧啶和盐酸麻黄碱分别在3.3~33.6μg.mL-1,6.0~60.7 5μg.mL-1峰面积和浓度呈线性关系,相关系数均为0.999 6,磺胺嘧啶和盐酸麻黄碱的平均回收率分别为101.1%和100.0%。以文献方法作为参考方法,通过F-检验核对了定量方法的精密性,磺胺嘧啶和盐酸麻黄碱的两方法平均偏差的比值均接近于1.0。结论该分析方法准确、稳定,可用于复方磺胺嘧啶滴鼻液的质量控制。     

HPLC法测定磺胺嘧啶麻黄碱滴鼻液的含量

目的建立一种同时测定磺胺嘧啶麻黄碱滴鼻液中磺胺嘧啶和盐酸麻黄碱含量的方法。方法采用Diamonsil C18色谱柱(150 mm×4.6 mm,5μm),流动相:缓冲液(0.01 mol.L-1磷酸二氢钾,0.5%三乙胺,磷酸调pH至2.8)-甲醇(80∶20,V/V),流速1mL.min-1,柱温25℃,检测波长256 nm。结果在该色谱条件下,盐酸麻黄碱和磺胺嘧啶的线性回归方程分别为y=796.30x+8.01(r=0.999 1,n=6)和y=69.04x-21.10(r=0.999 9,n=6)。加样回收率97%~103%(n=3),RSD<3%(n=3)。样品在8 h内稳定。测得样品中盐酸麻黄碱含量在97%~103%之间,磺胺嘧啶含量在90%~110%之间。结论该方法简便、快速、准确、重现性好。     

磺胺嘧啶麻黄碱滴鼻液定性定量方法研究

目的研究磺胺嘧啶麻黄碱滴鼻液的定性定量方法。方法采用化学反应法及HPLC法定性定量鉴别处方中的磺胺嘧啶及盐酸麻黄碱。采用HPLC法测定磺胺嘧啶及盐酸麻黄碱的含量,色谱柱为Hibar RP-18endcapped(150 mm×4.6 mm,5μm),流动相为磷酸盐缓冲液(p H值为3.0±0.1)-乙腈(90∶10),流速1.0m L?min-1,检测波长210 nm。结果化学反应和HPLC法均能定性鉴别磺胺嘧啶及盐酸麻黄碱。磺胺嘧啶和盐酸麻黄碱分离良好;进样浓度分别为99.96²99.88μg?m L-1(r=0.999 8,n=5)和19.86299.88μg?m L-1(r=0.999 8,n=5)和19.86⁵9.58μg?m L-1(r=0.999 9,n=5)与峰面积呈良好的线性关系。磺胺嘧啶和盐酸麻黄碱的平均回收率在98.0%59.58μg?m L-1(r=0.999 9,n=5)与峰面积呈良好的线性关系。磺胺嘧啶和盐酸麻黄碱的平均回收率在98.0%¹00%,RSD均<1.2%(n=3)。结论本方法简便、快速、准确,重复性好,可用于磺胺嘧啶麻黄碱滴鼻液的质量控制。     

复方磺胺嘧啶锌膜剂的制备及应用

对复方磺胺嘧啶膜剂的处方设计、制备方法、质量控制及临床应用进行了介绍。处方中主要成分：磺胺嘧啶、锌、地塞米松、盐酸达克罗宁。本制剂经过４５例口腔溃疡患者的疗效观察，总有效率达９５．５６％，本品具有显效迅速，作用持久，携带方便等优点。     

高效液相色谱法测定联磺甲氧苄啶片中3组份的含量

目的:建立采用高效液相色谱法(HPLC)测定联磺甲氧苄啶片中磺胺甲卟恶唑,磺胺嘧啶和甲氧苄啶的含量.方法:色谱柱为Diamonsil (TM) C18(5 μm, 200 mm×4.6 mm),流动相为乙腈∶水∶磷酸(50∶50∶0.1),每1000 mL流动相中加十二烷基硫酸钠3.5 g,流速1 mL*min-1,检测波长为257 nm.结果:磺胺甲卟恶唑、磺胺嘧啶和甲氧苄啶3种成分的回收率分别为99.78%,99.82%,99.90%.结论:方法简便,结果准确可靠.     

磺胺嘧啶出口分析

磺胺嘧啶为老牌抗菌药,问世至今已有近70年历史,我国生产磺胺嘧啶也有50余年历史。多年来,磺胺嘧啶一直是我国出口创汇的老牌原料药晶种,年出口量达3000余吨,年出口金额达2000多万美元。最近以来,我国磺胺嘧啶出口市场出现了一些新变化,主要表现在出口价格大幅上升,出口金额稳步走高,出口数量同比下降,引人关注.     

大力克--异丙嗪合剂的制备及质量控制

目的: 在小儿磺胺嘧啶合剂处方的基础上研制大力克--非那根合剂,并建立质量标准.方法: 用酸碱滴定法测定磺胺嘧啶的含量,用紫外分光光度法测定甲氧苄啶的含量.结果: 磺胺嘧啶、甲氧苄啶的平均回收率分别为99.76%和99.90%,RSD分别为0.29%和0.58%.结论: 该制剂配方合理,质量可控,可减少小儿用药次数,值得推广.     

HPLC同时测定复方磺棕合剂中的3种组分

目的 建立测定复方磺棕合剂中磺胺甲噁唑、磺胺嘧啶和甲氧苄胺嘧啶的方法.方法 采用HPLC法,色谱柱为Hypersil C18柱(200 mm×4.6 mm,5 μm),0.025 mol·L-1磷酸-乙腈(75:25)为流动相,检测波长220 nm.结果 磺胺甲噁唑、磺胺嘧啶和甲氧苄胺嘧啶的线性范围分别为0.10～2.00 μg(r＝0.9998)、0.10～2.00 μg(r＝0.9998)和0.02～0.40 μg(r＝0.9998),回收率分别为99.37%(RSD＝0.98%)、102.75%(RSD＝1.01%)和100.47%(RSD＝1.21%).结论 所建方法快速、简单、重复性好.     

不同酸度条件下茜素红-Al~(3+)-磺胺嘧啶体系的研究及应用

目的采用紫外分光光度法测定磺胺嘧啶的含量。方法磺胺嘧啶能使茜素红紫外吸收峰增强,但加入Al3+后,吸光度进一步增强。在pH4.50的B-R缓冲溶液体系中,于261nm处测定体系的吸光度;在pH10.00的B-R缓冲溶液体系中,于259nm处测定体系的吸光度,根据标准曲线计算磺胺嘧啶的含量。结果将此方法用于测定片剂和尿液中磺胺嘧啶的含量,结果与文献报道的荧光法一致。结论所用方法简单、快速、准确、灵敏。     

吸光度线性组合分光光度法测定呋磺胶囊的含量

目的:建立吸光度线性组合分光光度法测定呋磺胶囊中呋喃西林和磺胺嘧啶含量的方法.方法:应用吸光度线性组合分光光度法,不经分离直接测定呋磺胶囊中呋喃西林和磺胺嘧啶的含量.以260 nm、264 nm、375 nm为测定波长,分别在各点测定呋喃西林和磺胺嘧啶混合液的吸光度,通过线性组合计算磺胺嘧啶含量,用单波长测定呋喃西林含量.结果:平均回收率分别为99.98%、RSD=1.34%和99.94%、RSD=0.84%.结论:本方法简便、快捷,结果准确,适用于该制剂的质量分析检验.     

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.     

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.     

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.     

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,5 μm）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）对检测出色谱进行指纹图谱相似度评价。结果 建立了鼻渊净胶囊的HPLC指纹图谱,确定了20个共有峰,15个峰归属到各药材,其中5个峰确认了化学成分;10批样品的指纹图谱的整体相似度与对照图谱比较,均在90%以上。结论 所建立的鼻渊净胶囊指纹图谱有助于从整体上控制该制剂的质量。     

包公藤甲素类似物的合成

包公藤甲素(简称包甲素)系从包公藤茎中分离的一个新生物碱,其结构为2β-羟基-6β-乙酰氧基-N-去甲托品烷(1),为一强效M-胆碱受体激动剂,已用于青光眼治疗。项中等已报道了不同的合成方法,合成品为外消旋体,合成步骤长、收率很低。     

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.     

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.