建立了高效液相色谱法(HPLC)同时测定芩黄颗粒中黄芩苷和甘草酸的含量.采用Agilent Eclipse XDB-C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈-0.05％磷酸溶液为流动相,梯度洗脱,检测波长为252 nm,流速为1.0 mL/min.结果显示,黄芩苷和甘草酸的进样浓度分别在61.84～618.4、8.256～82.56μg/mL(R2=0.9999,0.9999)范围内与峰面积呈良好线性关系;精密度、重复性和稳定性试验的RSD均小于2.0％;平均加样回收率分别为100.0％、99.2％,回收率的RSD分别为1.0％、0.6％(n=6).本方法操作简便、准确,可用于芩黄颗粒中黄芩苷和甘草酸含量的同时测定.

对加米霉素合成工艺进行了优化.(E)-红霉素A肟在氢氧化锂存在下于异丙醇中经异构化得(Z)-红霉素A肟,以THF作溶剂,在冰水浴条件下与对甲苯磺酰氯的丙酮溶液反应,然后经异丙醇重结晶得重排产物9-脱氧-12-脱氧-9,12-亚胺醚-8a,9-二脱氢-8a-氮杂-8a-红霉素A,纯度90％.在甲醇-水中经硼氢化钠还原得9-脱氧-8a-氮杂-8a-同型红霉素A,纯度94％.最后在钯炭催化下与丙醛经还原烃化得目标化合物,纯度99.6％,总收率30.7％.优化后的工艺反应条件温和、操作便捷,且各中间体均采用重结晶精制,质量便于控制,适合工业化生产.

建立了加米霉素对照品的标定方法.采用紫外光谱、红外光谱、核磁共振波谱、质谱和X射线单晶衍射进行结构确认,高效液相色谱法进行纯度检查,质量平衡法进行定量分析,并采用定量核磁技术对赋值结果进行验证.结果显示,加米霉素对照品原料纯度为99.9％;质量平衡法赋值结果为98.8％,定量核磁共振法验证结果为98.3％.加米霉素对照品原料定量赋值结果准确、可靠,能够用于加米霉素原料及制剂的鉴别和含量测定.

[目的]建立用HPLC测定加米霉素含量的方法.[方法]采用高效液相色谱法,色谱柱为XBridge C18柱(250 mm×4.6 mm,5μm),流动相为磷酸盐缓冲液(取0.05 mol/L磷酸氢二钾溶液,用稀磷酸调节pH至8.0)-乙腈(30:70),流速为1.0 mL/min,柱温为30℃;检测波长为205 nm.[结果]加米霉素在0.4984～1.9936 mg/mL(r=0.9999)峰面积与浓度呈良好的线性关系,平均加样回收率为99.2％,RSD=0.6％.[结论]该方法重复性良好,能准确测定加米霉素的含量.

建立并验证了刺五加甘草颗粒中紫丁香苷含量的测定方法.采用高效液相色谱法,色谱柱为Agilent Zorbax SB-C18(250 mm×4.6 mm,5μm),流动相为乙腈-水梯度洗脱;检测波长为265 nm;流速为1.0 mL/min;柱温为30℃.试验结果表明紫丁香苷进样浓度在0.01218～0.08120 mg/mL范围内,与峰面积呈良好的线性关系(r=0.9999),加样回收率在96.46％～99.53％之间,平均回收率为98.4％(n=6),RSD为1.2％.试验建立的方法简便、准确度高、专属性强,可用于刺五加甘草颗粒中紫丁香苷含量的测定.

[目的]建立五加芪粉中总糖的含量测定方法,以控制五加芪粉的质量.[方法]采用苯酚-硫酸比色法,检测波长为494 nm,以无水葡萄糖为对照品对五加芪粉中总糖的含量进行测定.[结果]无水葡萄糖对照品溶液的线性范围为0.342～1.035 mg/mL(r=0.9994),平均加样回收率为98.5％,RSD=3.3％(n=6).[结论]该研究确定的方法简单、可靠、准确,可用于测定五加芪粉中总糖的含量.

为了考察苦参功劳颗粒治疗鸡大肠杆菌病的临床效果,按照入选标准挑选662只大肠杆菌病自然发病鸡只进行试验.将662只鸡随机分为3个组,3个组分别为苦参功劳颗粒试验组(300只)、四黄止痢颗粒对照组(300只)、感染对照组(62只).试验各组按推荐的临床给药途径和剂量进行给药,试验期间统计各组鸡群日均采食量、死亡率和给药组的治愈率.结果显示:苦参功劳颗粒按1.0g/L剂量饮水,连用5天,能减少大肠杆菌病引起的鸡只死亡,同时对疾病引起的采食量降低、生长发育受阻具有改善作用.结论:本试验为苦参功劳颗粒的临床应用提供了数据支持,同时建立了鸡大肠杆菌病的病例入选标准、疗效判定标准,为新兽药的临床评价提供参考方法.

To establish the method for determining of astragaloside in Wujiaqi powder by HPLC-ELSD, C18 column (Kromasil 100-5C18, 150 mm×4.6 mm, 5μm)was used with the mobile phase consisted of acetonitrile-water (35∶65), the flow rate was 1.0 mL/min, column temperature was 30 ℃, Evaporative light scattering detection condition: drift tube temperature was 60 ℃, spray tube temperature was 36 ℃, the nitrogen pressure was 25 psi.The calibration curve was linear at a range of 1.524～10.16 μg for astragaloside (r=0.9991), the average recovery was 99.4％ and RSD was 4.6％(n=6).The method was accurate with a good reproducibility and can be used as a quantitative analysis of astragloside in Wujiaqi powder.

To evaluate the pharmacokinetics and bioequivalence of two kinds of ivermectin injections in rabbits,in a randomized two -way self -crossover study,16 healthy rabbits were randomly divided into two groups,and were given respectively a single dose of two kinds of ivermectin injection by subcutaneous injection (5 mg/kg).Plasma concentrations of ivermectin were measured by HPLC.The pharmacokinetic parameters were calculated by 3P97 pharmacokinetic software,and the bioequivalence were evaluated.The main pharmacokinetic parameters of the test and reference preparations were as follows:Tmax were (26.45 ±8.62)h,(22.33 ±11.72)h;Cmax were (182.73 ± 59.27)ng/mL,(166.77 ±65.25)ng/mL;AUC0 -t were (21122 ±9999)ng·h·L -1 ,(19475 ±7009)ng·h·L -1;AUC0 -∞were (27390 ±12197)ng·h·L -1 ,(31559 ±13412)ng·h·L -1 .The pharmacokinetic parameters (AUC0 -t、AUC0 -∞、Cmax、Tmax ) showed no significant difference between test and reference preparations of ivermectin injections.The test and reference formulations were bioequivalent after two one -side t -test.This study provided theoretical basis for making of veterinary clinical dosage regimen and clinical rational administration.

The pharmacokinetics and relative bioavailability of the ceftiofur injection and RTUEZ sterile suspension were investigated in pigs.Ten pigs received 5mg/kg of ceftiofur injection by(i.m,Huizhong,China)and ten pigs injected the same closage of RTUEZ(i.m,Pfizer,USA).Blood samples were collected and analysed by high-performance liquid chromatography(HPLC).Pharmacokinetics parameters were estimated using the WinNonlin5.2.1software package and SPSS16.0analysis of the time and concentration data.The main pharmacokinetics parameters for ceftiofur injection(Huizhong,China)and RTUEZ sterile suspension(Pfizer,USA)administrated intramuscularly were as follows:Tmax:(2.63±0.74),(3.38±1.92)h;Cmax:(14.06±2.21),(9.48±1.84)mg/L;t1/2β:(17.65±2.07),(17.70±2.43)h;MRT:(23.21±2.68),(22.11±2.50)h;AUClast:(240.81±47.73),(182.51±36.12)μg·h·mL-1,respectively.Comparing cefiofur injection with RTUEZ sterile suspension,statistical analysis on plasma showed that the pharmacokinetic parameters of Cmaxand AUClastwere different significantly(P0.01).It indicated that ceftiofur injection was absorbed quickly and completely,with highly bioavailable.The relative bioavailability of cefiofur injection following i.m.administration was 132%,better than that of RTVEZ sterile suspension.The results demonstrated that ceftiofur injection(Huizhong,China)was absorbed quickly and completely,with highly peak concentration and bioavailability.

本试验选用健康母猪及所产仔猪,随机分为4组,各组按照保健方案给药,并持续观察至断奶后7天,以增重和发病率为指标,观察10%恩诺沙星注射液对哺乳及断奶仔猪预防保健效果。结果表明,试验组和药物对照Ⅰ组在试验结束的净增重显著高于药物对照Ⅱ组(P<0.05),试验组和药物对照Ⅰ组的发病率显著低于药物对照Ⅱ组(P<0.05),而两个试验组之间差异不显著(P>0.05)。该试验为10%恩诺沙星注射液作为仔猪保健用药提供了参考数据。

为考察苦参苍术口服液对鸡耐药大肠杆菌的临床应用效果,对其进行了临床疗效试验。试验结果表明:1L饮水中添加苦参苍术口服液1mL~2mL,连用5天,能明显降低鸡人工感染耐药大肠杆菌病引起的死亡率,且对人工感染大肠杆菌引起的鸡只生长发育受阻有一定程度的改善作用。苦参苍术口服液与乳酸诺氟沙星联合使用时,疗效明显增强,与乳酸诺氟沙星阳性对照组相比,发病率明显降低(p<0.01),有效率明显升高(p<0.01)。

<正>生物医药产业是关系国民健康的重要高新技术产业,也是我国在"十二五"时期要大力发展的战略性新兴产业的重要组成部分。我国在天然药物开发与利用方面具有悠久的历史和丰富的资源,尤其是在毒素生物资源作为药物的研究与利用方面有较好的基础。

Five compounds were isolated from ethyl acetate extraction from ethanol extraction of stems and leaves of Mahonia fortunei,and purified by silica-gel and sephadex column chromatography.The structures of the compounds were determined by physicochemical properties and spectrum analysis(TLC,1H NMR,13C NMR,MS).Five compounds were identified as berberine(Ⅰ),jatrorrhizine(Ⅱ),5'-Methoxyhydnocarpin-D(Ⅲ),lutelin(Ⅳ) and β-sitosterol(Ⅴ).5'-Methoxyhydnocarpin-D(Ⅲ) was isolated and identified from this plant for the first time.

In order to observe the applied reliability of Shuanghuanglian oral liquid, the experiment was conducted in accordance with acute toxicity requirements in compilation of veterinary drug registration data. The acute toxicity of Shuanghuanglian oral liquid was studied by selecting mouse in this Shuanghuanglian oral liquid was demonstrated by the minimal lethal dose and the showed that 138.2 times experiment, the toxicity of LD50 of mouse. The results the minimal lethal dose ranged between 49.2 and 60.8 g/kg, which was equivalent to from 111.8 to of daily dosage of poultry. Shuanghuanglian oral liquid was relatively safe in clinical application.

Three groups of swine(n=5) were injected intramuscularly Baytril 5%,enrofloxacin injection A,and enrofloxacin iniejction B.Plasma concentration was measured by HPLC,and concentration-time data was processed by Winnonlin6.1.The results showed that models of all groups were best fit by one-compartment open model with peak concentration of 0.87,0.63,0.49 μg/mL,and AUC of 6.32,5.31,3.45 h·μg·mL-1.Baytil 5% is the best in pharmacokinetics,then injection B,injection A last.It indicated that injection B was improved significantly,but slightly inferior to Baytril 5%.Its pharmacokinetic attribute of absorption should be improved.

Researches on the physicochemical identification and thin layer chromatography(TLC) identification of Rhizoma atractylodis from different regions were carried out.The results showed that Rhizoma atractylodis from different regions had different identification features.Conclusion of the above-mentioned research is useful for the application and quality standard establishment of Rhizoma atractylodis.

采用人工接种孢子化柔嫩艾美耳球虫卵囊的方法.复制鸡球虫病,观察并计算球速杀饮水剂对人工感染柔嫩艾美耳球虫病鸡的死亡率、增重率、血便记分、盲肠病变记分和卵囊值的影响,并求出球速杀饮水剂的抗球虫指数(ACI),依据农业部1992年<实验临床试验技术规范>对洛阳惠中兽药有限公司生产的球速杀饮水剂对人工感染鸡球虫病的疗效进行临床试验.试验结果表明:球速杀饮水剂按每1 L水1 g混饮,连用3 d,能提高球虫病鸡的存活率和相对增重率,减少血便记分和盲肠内容物卵囊数,减轻盲肠病变并对鸡柔嫩艾美耳球虫病有一定的防治作用.

依据农业部1992年《实验临床试验技术规范》的要求,对洛阳惠中兽药有限公司生产的硫酸头孢喹肟注射液对实验性仔猪大肠杆菌病进行临床治疗试验。采用人工接种大肠杆菌的方法,复制仔猪大肠杆菌病,按推荐的临床给药途径给药,给药后观察动物的生理状况与发病情况,记录死亡数,分治愈、显效、有效、无效等指标对结果进行统计并评价。结果表明:硫酸头孢喹肟注射液按每1kg体重2mg肌注,一日一次,连用3d,对仔猪大肠杆菌可取得良好的效果。

受洛阳惠中兽药有限公司的委托,河南省兽药工程技术研究中心对芩黄颗粒进行了人工感染鸡传染性支气管炎(IB)的临床防治试验.采用人工接种传染性支气管炎的方法,复制鸡传染性支气管炎病,按推荐的临床给药途径给药,经预防给药后观察动物的发病情况,并按显效、有效、无效等疗效判定指标对结果进行统计并评价.试验结果表明:芩黄颗粒按每1 L水1 g混饮,连用3 d,对鸡传染性支气管炎有良好的预防效果.