甲苯咪唑国家对照品的研制

以精制后的甲苯咪唑为原料研制甲苯咪唑国家对照品,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...     

乙酰氨基阿维菌素国家对照品的研制

以乙酰氨基阿维菌素为原料研制首批乙酰氨基阿维菌素国家对照品,并进行质量评价。采用高效液相色谱法和质谱法对原料进行结构确证,分装后的乙酰氨基阿维菌素对照品采用质量平衡法定值,同时采用高效液相色谱外标法加以佐证。结果显示,以质量平衡法计算乙酰氨基阿维菌素(B_1a+B_1b)含量为97.79%,液相色谱外标法测定含量为98.18%,两种方法测定结果基本一致。本次研制的乙酰氨基阿维菌素对照品可用于乙酰氨基阿维菌素及其制剂的鉴别与含量测定。     

匹莫苯丹对照品的定值研究

为了研制匹莫苯丹对照品,采用精制后的匹莫苯丹为原料,并进行质量评价。采用熔点法、红外分光光度法、液相色谱法对原料进行鉴别,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,以质量平衡法计算其含量为99.8%,容量法测定含量为99.7%,液相色谱外标法测定含量为99.6%,三种方法测定结果一致。本次研制的匹莫苯丹对照品可用于匹莫苯丹及其制剂的鉴别与含量测定。     

注射用氨苄西林钠氯唑西林钠含量测定

建立反相高效液相色谱法测定注射用氨苄西林钠氯唑西林钠中氨苄西林钠和氯唑西林钠的含量。方法:采用奥泰公司C18色谱柱(250mm×4.6mm,5μm),磷酸盐缓冲液磷酸-甲醇-磷酸(85:15:0.01),检测波长为225nm,流速为1.0ml/min,柱温为30℃。氨苄西林钠在20~160μg·m L-1,氯唑西林钠在25-200μg·m L-1范围内呈良好的线性关系。氨苄西林钠和氯唑西林钠平均回收率分别为99.56%、99.63%。结论:本法简便、准确,可用于注射用氨苄西林钠氯唑西林钠中氨苄西林钠和氯唑西林钠的含量测定。     

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。     

高效液相色谱法测定苄星邻氯青霉素乳房注入剂中苄星邻氯青霉素的含量

用反相高效液相色谱法测定苄星邻氯青霉素乳房注入剂中苄星邻氯青霉素的含量。采用AgilentEclipseXDB-C185μm4.6×150mm色谱柱;流动相为0.1mol/L磷酸二氢钠-乙腈(3:1);检测波长为220nm;柱温为40℃。在该色谱条件下,苄星邻氯青霉素在20μg/ml～180μg/ml浓度范围内线性关系良好,相关系数r=0.99999;100%浓度时平均回收率为100.7%,RSD=0.04%。该方法快速灵敏,准确实用。     

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。     

奶牛饲养允许使用的抗菌药及其使用规定

药名制剂用法与用量(用量以有效成分计)休药期氨苄西林钠ampicillin sodium氨苄西林钠+氯唑西林钠(干乳期)ampicillin sodium+cloxacillin sodium(dry cow)氨苄西林钠+氯唑西林钠(泌乳期)smpicillin sodium+cloxacillin sodium (milking cow)苄星青霉素benzathine benzylpenicillin苄星邻氯青霉素benzathine cloxacillin青霉素钾(钠)benzy1penicillin prtassium硫酸小檗碱berberine sulfate头孢氨苄cefalexin氯唑西林钠cloxacillin sodium恩诺沙星enroflixacin乳糖酸红霉素erythromycin lactobionate土霉素oxytetracycline盐酸…     

杨树花口服液的质量标准研究

本试验采用薄层色谱法鉴别杨树花口服液中3种有效成分(芹菜素、木犀草素和槲皮素);以芹菜素为对照品,采用紫外可见分光光度法测定其中的总黄酮含量,并采用高效液相色谱法测定其中木犀草素的含量,通过研究确定了对杨树花口服液质量检测的简单、准确的分析方法,进一步完善了杨树花口服液的质量标准。     

盐酸阿苯达唑亚砜对照品候选物纯度检测方法的建立

以盐酸阿苯达唑亚砜原料为基础,通过反复提纯,得到盐酸阿苯达唑亚砜对照品候选物,该候选物经过熔点,薄层色谱法（TLC）和高效液相色谱法检测,初步确认符合对照品的要求,经过高效液相色谱检测,采用面积归一化法计算其纯度不小于99.5%。该方法的建立为盐酸阿苯达唑对照品进一步研究提供了帮助。     

Ocular and serum disposition kinetics of cloxacillin after topical administration of benzathine cloxacillin and intravenous administration of sodium cloxacillin to calves

Disposition kinetics of cloxacillin were examined in calves after topical administration of benzathine cloxacillin and single IV administration of sodium cloxacillin, and the susceptibility of 17 field isolates of Moraxella bovis was measured. For the IV pharmacokinetic phase, sodium cloxacillin was administered at dosage of 10 mg/kg of body weight to male Holstein calves (n = 6, weighing 146 to 170 kg), and serum concentration of cloxacillin was measured thereafter for 10 hours. For the ocular pharmacokinetic phase, 6 calves were given either of 4 benzathine cloxacillin topical formulations consisting of 50-, 125-, 250-, or 375-mg doses. Treatment was repeated every 10 days until all 4 benzathine cloxacillin dosages were tested in the same 6 calves. Blood and tears were collected for 72 hours after each benzathine cloxacillin formulation was administered, and the concentration of cloxacillin in each specimen was measured, using a bioassay. The minimal inhibitory concentration of cloxacillin for 17 field isolates of M bovis was determined by use of an agar pour-plate dilution assay. After single IV administration of sodium cloxacillin, its half-life, body clearance, and volume of distribution were 19.5 +/- 12.8 minutes, 18.3 +/- 2.2 ml/min.kg, and 496 +/- 290 ml/kg, respectively. After topical administration of benzathine cloxacillin, cloxacillin concentration in lacrimal fluid peaked between 30 and 45 minutes and ranged between 963 micrograms/ml and 3,256 micrograms/ml for the 125- and 375-mg doses, respectively. There was no detectable cloxacillin activity in the lacrimal fluid of any calf by 36 hours after topical administration of benzathine cloxacillin, and cloxacillin was not detected in the serum at any time.(ABSTRACT TRUNCATED AT 250 WORDS)     

Topically applied benzathine cloxacillin for treatment of experimentally induced infectious bovine keratoconjunctivitis

The efficacy of an ophthalmic ointment containing benzathine cloxacillin for treatment of infectious bovine keratoconjunctivitis was determined in 2 experiments. In the first experiment, Holstein calves (n = 6/group) were inoculated with Moraxella bovis and treated on postinoculation days 3 and 6 with either topically applied benzathine cloxacillin (250 mg/eye) or long-acting oxytetracycline formulation (20 mg/kg of body weight, IM). A third group of inoculated calves remained untreated as controls. For the second experiment, 4 groups of calves (n = 6/group) were inoculated and treated on postinoculation days 3 and 6 with 50, 125, 250, or 375 mg of benzathine cloxacillin; a fifth untreated group served as controls. Ocular specimens were obtained for microbiologic culture, and eyes were observed and assigned a clinical score daily. Eyes were photographed on alternate days. Ulcer surface area was measured, using a planimeter. In experiment 1, the week-2 ulcer surface area measurements for both groups of treated calves were smaller than those for controls. There was a greater frequency of M bovis isolation from the ocular secretions of controls than from those of benzathine cloxacillin-treated calves during postinoculation weeks 2 and 3. The number of M bovis isolations from the benzathine cloxacillin- and oxytetracycline-treated calves was not significantly different at any sample collection interval. On week 3, the scores of the benzathine cloxacillin-treated calves were smaller than those of controls. In experiment 2, calves of the 250- and 375-mg groups had smaller ulcer surface area measurements than did controls on week 2. By week 3, calves of the 375-mg group had smaller scores than did controls.(ABSTRACT TRUNCATED AT 250 WORDS)     

Effectiveness of two benzathine cloxacillin formulations for treatment of naturally occurring infectious bovine keratoconjunctivitis

A field study was performed to determine the effectiveness of benzathine cloxacillin for the treatment of infectious bovine keratoconjunctivitis in cattle from 2 farms located in northern California. The study was performed between June and September of 1987. Affected calves ranging from 2 to 9 months of age were selected from the main herd when signs of corneal ulceration were observed. The study was conducted in 2 phases. For phase I, the affected calves of herd 1 (n = 21; Holsteins) and herd 2 (n = 43 Angus crossbred), were randomly assigned to 1 of 3 groups, and were either treated with 250 (n = 23) or 375 mg (n = 21) of benzathine cloxacillin, or mineral oil (n = 20) on days 1 and 4. For phase II, affected calves (n = 16; Angus crossbred, 3 to 9 months of age) from herd 2 were treated with benzathine cloxacillin (250 mg). Eight of these calves were retreated on day 4. After treatment, all calves were examined every 72 hours for 16 days. For examinations, a clinical score was assigned to each eye, and the surface areas of photographed corneal ulcers were measured. The ocular secretions were collected and examined culturally for Moraxella bovis. On days 7, 10, and 13, the calves treated with benzathine cloxacillin had significantly (P less than 0.05) lower lesion scores, compared with the controls.(ABSTRACT TRUNCATED AT 250 WORDS)     

苄星氯唑西林乳房注入剂无菌检查方法研究

本试验旨在建立苄星氯唑西林乳房注入剂无菌检查法并进行验证.采用离心—薄膜过滤—酶中和相结合的方法,按照《中国兽药典》2010年版一部附录进行试验.结果显示采用离心—薄膜过滤—酶中和相结合的方法,以0.5%聚山梨酯-80 pH 7.0氯化钠—蛋白胨缓冲液冲洗,冲洗量400 mL/膜,在最后的培养基中加入不少于300万单位的青霉素酶可有效消除样品对各试验菌株的抗菌活性;验证试验结果显示各验证菌生长良好,各供试品管均未见菌生长.结果表明本试验成功建立了可靠、准确、可用于苄星氯唑西林乳房注入剂的无菌检查法.     

Influence of the genotype of Staphylococcus aureus, determined by pulsed-field gel electrophoresis, on dry-period elimination of subclinical mastitis in Canadian dairy herds

By combining information from 2 databases, we investigated the possibility of an association between the genotype of Staphylococcus aureus causing bovine intramammary infection and dry-period cure of subclinical infection. The 1st database contained bacteriologic and cow data from a field study evaluating the efficacy in such infections of a new intramammary dry-cow therapy (DCT) containing tilmicosin phosphate, in comparison with a commercially available DCT containing benzathine cloxacillin. Isolates of S. aureus from that study were frozen and later independently analyzed by pulsed-field gel electrophoresis (PFGE) and macrorestriction DNA fingerprinting. The molecular information, summarized and published elsewhere, constituted the 2nd database. Data from 121 subclinically infected quarters of 92 cows from 40 herds were studied by univariate and multivariable regression analysis. Infection by an isolate of PFGE lineage group D was more likely than infection by an isolate of group A or F to be cured (P < 0.05). Cows infected by lineage group D had a higher linear somatic cell count score (LS) from the last Dairy Herd Improvement test before the dry period than did cows infected by the other lineage groups (P = 0.04). Although the probability of cure was significantly lower for cows with an LS at or above the mean of 5.7 for the study population (P = 0.05), when such a cow was infected with lineage group D, cure was significantly more likely (P < 0.001) than when it was infected by another lineage group. Significantly more (P = 0.02) of the infections treated with tilmicosin (74%) than of those treated with benzathine cloxacillin (53%) were cured, and significantly more (P = 0.05) of the infections by group D (81%) than of those by group A (57%) or group F (54%) were cured. However, there was no difference in cure rate for any PFGE genotype when tilmicosin phosphate was administered; when benzathine cloxacillin was administered, 87% of lineage group D isolates were eliminated, as compared with 46% of group A and 33% of group F isolates (P < 0.05). This research demonstrates that certain genotypes of S. aureus may naturally elicit a greater inflammatory response, yet be more susceptible to elimination by antibiotics in the dry period, than other genotypes.