苯甲磺酰截短侧耳素国家对照品的研制

研制首批苯甲磺酰截短侧耳素甲磺酰截短侧耳素对照品为白色或类白色粉末,红外光吸收图谱与USP溯源对照品图谱一致,质谱法测定分子离子峰为555.19 Da([M+Na]~+),高效液相色谱法测定其平均纯度为99.7%,可作为系统适用性对照品,用于延胡索酸泰妙菌素及其制剂含量测定的系统使用性检查。     

马拉硫磷对照品的制备

通过对马拉硫磷对照品候选物进行全面质量控制,以美国药典委员会提供的马拉硫磷对照品作为溯源对照品,用高效液相方法通过协作标定对制备的马拉硫磷对照品进行定值,确定制备马拉硫磷对照品含量为99.0%,相对标准偏差为0.3%。通过对马拉硫磷对照品的研制,期望能对兽用化学药品对照品的研制提供一些参考意见和建议。     

复方阿莫西林乳房注入剂无菌检查方法的确立

建立了复方阿莫西林乳房注入剂的无菌检查方法。根据《中国兽药典》2010年版一部附录要求,通过比较薄膜过滤法和直接加入法对本品的适用性,最终选用直接加入法作为无菌检查方法,即以每1 mg阿莫西林中加入9000单位的青霉素酶来消除供试品的抑菌活性,并通过无菌方法验证,证明该方法适用于对复方阿莫西林乳房注入剂进行无菌检查。     

安替比林对照品纯度控制方法的试验

采用薄层层析对安替比林对照品的纯度测定方法进行了研究。用薄层层析进行半定量分析，杂质控制在０．１％以下，从而进一步完善了安替比林对照品内在质量控制     

泰拉霉素国家对照品的标定研究

为了有效控制泰拉霉素原料及注射液的产品质量,研制了泰拉霉素国家对照品。采用精制后的泰拉霉素为原料进行本批对照品的研制,原料分装后进行质量检测及均匀性评价,并标定含量。采用红外分光光度法、费休氏水分测定法等对其进行理化分析,利用高效液相色谱法进行有关物质测定及均匀性检验,采用质量平衡法进行标准物质含量计算,并通过差示扫描量热法对质量平衡法的准确性进行验证。研制的泰拉霉素国家对照品的含量为98.3%,采用多种不同方法对本品进行定性与定量研究,确保了国家标准物质标定结果的准确性。本对照品可用于泰拉霉素原料及注射液的鉴别与含量测定,对于提高和保证兽药产品质量具有重要意义。     

国际化学对照品的研制指导原则介绍

根据世界卫生组织对国际化学对照品（ICRS）的研制指导原则,从国际化学对照品的建立前提、原料选择、测定方法、含量赋值、分装、贮存、稳定性监测和有效期规定等7个方面对对照品的研制要求作了简要介绍。     

头孢噻呋对照品的研制

按照国家对照品的研制指导原则,进行了头孢噻呋国家对照品的研制。通过稳定性研究,确定了盐酸头孢噻呋作为对照品原料,然后对所选取原料分别用元素分析、红外分光光度法和液相色谱法确证了头孢噻呋的结构。液相色谱法测定纯度为96．8％,含量赋值为87．5％。     

阿莫西林脂质体的制备及质量评价

采用薄膜分散法制备阿莫西林脂质体,以粒径和包封率为指标评价其质量.前期以正交设计优化筛选出最佳制备工艺,以最优工艺制备阿莫西林脂质体,测定其平均粒径和包封率.实验所制得的脂质体的平均粒径为114.6 nm,包封率为64.89％.结果表明,采用薄膜分散法制备阿莫西林脂质体的方法可行,阿莫西林脂质体的制备为兽药新剂型的研究与应用提供了有价值的参考.     

烯丙孕素对照品的研制及标定

研制了烯丙孕素对照品并对其进行标定。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,并用核磁共振波谱法对赋值结果进行验证。结果显示,烯丙孕素对照品原料纯度为99.96%;质量平衡法赋值结果为99.92%,定量核磁共振法验证结果为99.60%。烯丙孕素工作对照品定量赋值结果准确、可靠,能够用于烯丙孕素原料及制剂的鉴别和含量测定。     

甲苯咪唑国家对照品的研制

为了研制甲苯咪唑国家对照品,采用精制后的甲苯咪唑为原料,并进行质量评价。采用紫外分光光度法、红外分光光度法对原料进行鉴别,采用质量平衡法定值,同时采用容量法和高效液相色谱法加以佐证。结果显示,紫外吸收图谱与标准规定一致、红外光吸收图谱与USP溯源对照品图谱一致;以质量平衡法计算其含量为99.8%,容量法测定含量为99.9%,液相色谱外标法测定含量为99.9%,三种方法测定结果一致。本次研制的甲苯咪唑对照品可用于甲苯咪唑及其制剂的鉴别与含量测定。     

Relative oral bioavailability of microgranulated amoxicillin in pigs

A new microgranulated formulation of amoxicillin trihydrate for in-feed medication was developed using a lipogelled matrix. Its relative bioavailability was compared with powdered drug in pigs and an assessment was made to determine whether therapeutic concentrations were achieved. Microgranules containing 10% (MICR10) and 30% (MICR30) amoxicillin and free amoxicillin trihydrate powder (reference, AMX) were administered at dosages of 50 mg of amoxicillin/kg b.w. using a three-way-crossover design. Amoxicillin analysis in serum was performed by a sensitive high performance liquid chromatography (HPLC) method with fluorometric detection, using an extraction procedure already described for edible tissues of fish and adapted and validated for pig serum. The oral bioavailability of both microgranulated formulations was higher than that of the reference formulation [relative bioavailability (F): 153.9 +/- 58.2% for MICR10; 126.2 +/- 70.5% for MICR30] and the area under the concentration-time curve (AUC) values of MICR10 and AMX formulations were significantly different (P < 0.05). Differences between the mean maximum concentration (Cmax), time of Cmax (tmax) and mean residence time (MRT) of the drug formulations were not significant. Microgranulated amoxicillin is suitable for in-feed administration to pigs and, because of its higher oral bioavailability compared with the powdered compound, it may be more effective for the treatment of susceptible infections.     

Determination of Pinoresinol Diglucoside in Eucommie ulmoides Immunoenhancement Liquids by RP-HPLC

The assay was aimed to determine the content of pinoresinol diglucoside (PDG) in Eucommie ulmoides immunoenhancement liquids. The chromatographic conditions were as follows:Inersustain^® C18 column (250 mm×4.6 mm,5 μm) was under column temperature of 35℃, the mobile phase consisted of acetonitrile-0.2% phosphoric acid(15:85)with a flow rate of 1.0 mL/min,and the UV detection wavelength was 277 nm. Ethyl acetate was used as extraction solvent. In order to determine PDG of the test solution under the chromatographic conditions, the number of theoretical plates and resolution were used as system suitability indicators. Linear regression on reference substance (PDG),linearity range and the precision, stability, and reproducibility of the analysis method, the recovery test of adding samples were all determined. The results showed that under the content determination method, the number of theoretical plates of PDG in the test solution was 8 588, and the resolution was 3.046. PDG performed good linear relation at the linear range between 6 and 192 μg/mL, and the related coefficient was 0.9996. The precision experiments showed that the relative standard deviation (RSD) of reference substance solution was 0.74%. The RSD of reproducibility and stability of PDG in the test solution was 4.50% and 2.69%, respectively. The average recovery was 98.74% with RSD 0.65% (n=9). Under the chromatographic conditions established above, the contents of PDG in the test sample were between 0.124 and 0.127 mg/mL. The conclusion was that the RP-HPLC method performed well system suitability, precision, reoroducibility, stability, and high recovery rate. Meanwhile this method was quick, simple and reliable. It could be used to determine the content of PDG in Eucommie ulmoides immunoenhancement liquids.     

RP-HPLC法测定杜仲增免液中松脂醇二葡萄糖苷的含量

试验旨在建立测定杜仲增免液中松脂醇二葡萄糖苷含量的RP-HPLC法。以Inersustain^® C18（250 mm×4.6 mm,5 μm）为色谱柱,乙腈-0.2%磷酸（15：85）为流动相,流速1.0 mL/min,柱温35℃,紫外检测波长277 nm。以乙酸乙酯作为提取溶剂,在所建立的色谱条件下测定供试品溶液,以理论塔板数和分离度作为系统适用性指标。对对照品松脂醇二葡萄糖苷溶液进行线性回归,确定线性范围,考察分析方法的精密度、稳定性、重现性,并进行加样回收试验。结果显示,用所建立的方法测定供试品溶液中松酯醇二葡萄糖苷理论塔板数为8 588,分离度为3.046。松脂醇二葡萄糖苷对照品溶液在6~192 μg/mL浓度范围内线性关系良好,相关系数为0.9996;精密度试验结果显示松脂醇二葡萄糖苷对照品溶液峰面积相对标准偏差（relative standard deviation,RSD）为0.74%;重现性和稳定性试验结果显示供试品溶液中松酯醇二葡萄糖苷峰面积RSD分别为4.50%和2.69%;平均加样回收率为98.74%,RSD为0.65%（n=9）;在所建立的色谱条件下,供试品中松脂醇二葡萄糖苷的平均含量为0.124~0.127 mg/mL。结果表明,应用该方法测定杜仲增免液中松脂醇二葡萄糖苷的含量,系统适用性好,精密度高,重现性和稳定性好,回收率高,快速简便、准确可靠,可作为杜仲增免液中松脂醇二葡萄糖苷含量测定方法。     

Methoxydextran as an indicator of gastrointestinal transit in Japanese quail

The recovery of polyethylene glycol, a substance frequently used as an indicator of the dynamics in the liquid phase of intestinal chyme, is considerably influenced by the presence of trichloroacetic acid in certain applications. The suitability of (methoxy-14C)methoxydextrane as an intestinal indicator in the Japanese quail was tested in the study. After the administration of this indicator, the bird expires less than 1% of the substance in form of 14CO2. The recovery of labelled methoxydextrane is 98 +/- 7%. The distribution of the indicator within the segments of the gastrointestinal tract does not differ significantly from the distribution of (14C)polyethylene glycol 4000, measured in the absence of trichloroacetic acid. The transit of the labelled methoxydextrane into the jejunum did not reduce the radio-chemical purity of the isotope, as compared with its original purity before administration. A slight decrease was only recorded during the measurement of the cumulative excretion of the indicator for 72 hours, but this decrease has no influence upon the suitability of methoxydextrane as an intestinal indicator. (Methoxy-14C)methoxydextrane does not interact with trichloroacetic acid, whereas when polyethylene glycol is used as an indicator, the substance precipitates from the liquid phase just at the concentration commonly used for the removal of protein from biological samples.     

Acaricidal activity of kupetaba, a ground mixture of natural products, against Rhipicephalus appendiculatus

Eight substances were screened for the purpose of selecting a natural product as an acaricide for use within an integrated tick management system. One substance proved to be effective as an acaricide against all stages of Rhipicephalus appendiculatus and was named 'kupetaba'. It is a ground mixture of dried tobacco leaves (family Solanaceae) and a mineral called 'Magadi soda' which is mined around Lake Magadi in the Rift Valley province of Kenya. Investigation showed that kupetaba is commonly sold in local markets in East, West and Central Africa, where it is used for many purposes. The substance prevented the completion of all feeding phases of the tick, suppressed the oviposition capacity of the engorged ticks and drastically reduced the hatchability of the eggs. Larvae and nymphs were killed within 24 h of the application of the substance on calves' ears, while large numbers of adult ticks were also killed within 2-3 days of application during in vitro experiments. The suitability of the natural product as a local acaricide which resource-poor farmers in Africa can use to replace commercial acaricides within an integrated tick management system is discussed.     

钛白副产绿矾制备饲料级硫酸亚铁的工艺与生产

此文研究以钛白副产绿矾为原料,经酸浸、还原、絮凝除去杂质离子制得精制硫酸亚铁溶液,再经过滤、冷冻结晶、洗涤、真空干燥制备饲料级硫酸亚铁产品的新工艺,重点考察了精制工艺对产品质量的影响。结果表明：采用30%的硫酸溶液浸取、铁屑还原、投加0.1%PAM的条件下,可获得精制的硫酸亚铁溶液,对溶液进行冷冻结晶和真空干燥可制备达到HG/T2935-2000标准的饲料级硫酸亚铁产品。应用该工艺建成了一套10000t/a的生产装置,装置运行表明：原料成本低、经济效益好。     

复方淫羊藿散的薄层色谱鉴别

建立复方淫羊藿散的质量控制标准,采用薄层色谱法对复方淫羊藿散中的淫羊藿、女贞子、白术、茯苓进行定性鉴定。试验结果表明,淫羊藿、女贞子、茯苓的指标成分在与对照品或对照药材色谱相应位置上有相同的斑点,阴性对照无干扰。该方法专属性好、结果准确、重复性高,为复方淫羊藿散的质量控制建立了定性鉴别方法。     

Field evaluation of efficacy and tolerance of a 2% marbofloxacin injectable solution for the treatment of respiratory disease in fattening pigs

In a controlled and randomized field trial carried out in three European countries, 219 fattening pigs, from seven farms with respiratory disease problems, were treated intramuscularly for three or five days either with marbofloxacin 2 mg/kg/day, or with amoxicillin 7 mg/kg/day. Pigs were monitored daily until D5 (Day 5) and again at D21, and were weighed at D0 and D21. Pasteurella multocida, Actinobacillus pleuropneumoniae, and Mycoplasma hyopneumoniae were mainly identified in the pig lungs. The difference in the cure rate (74.5% in marbofloxacin group versus 68% in the amoxicillin group) was not significant. Mean rectal temperature was significantly lower after treatment with marbofloxacin. Other criteria tended to be favourable for the marbofloxacin group, although differences were not significant. The time to cure tended to be shorter for the marbofloxacin group (24.3% of pigs at 24 hours post-treatment versus 12.1% in the amoxicillin group). Marbofloxacin and amoxicillin relapse rates were 11.9% and 17.2% respectively (not significant) and daily weight gain was 746 g in the marbofloxacin group versus 687 g in the amoxicillin group (not significant). The 2% marbofloxacin solution was significantly better tolerated than amoxicillin.     

寒痢宁口服液的薄层鉴别

为了建立寒痢宁口服液的质量控制标准,采用薄层色谱法对寒痢宁口服液中的黄连、厚朴、陈皮、补骨脂进行定性鉴定。试验结果表明,黄连、厚朴、陈皮和补骨脂的特征成分在与对照品和对照药材色谱相应位置上显相同颜色的斑点,阴性对照无干扰。该方法专属性强,稳定性和重现性好,为寒痢宁口服液的质量控制建立了定性鉴定方法。