HPLC法同时测定复方磺胺间甲氧嘧啶注射液中磺胺间甲氧嘧啶钠和甲氧苄啶含量

利用高效液相色谱法(HPLC)同时测定复方磺胺间甲氧嘧啶钠注射液中磺胺间甲氧嘧啶钠和甲氧苄啶的含量。采用C₁₈柱(5μm, 4.6 mm×250.0 mm),以乙腈∶0.1%磷酸溶液(20∶80,V/V)为流动相，检测波长230 nm,柱温30℃,流速1.0 mL/min。结果表明，磺胺间甲氧嘧啶在5.00～200.00μg/mL浓度范围内与峰面积线性关系良好(R²=0.999 6),平均回收率为99.49%,RSD为0.18%;甲氧苄啶在1.00～50.00μg/mL浓度范围内与峰面积线性关系良好(R²=0.999 7),平均回收率为99.02%,RSD为0.60%。本方法简单快捷，精密度好，可用于控制复方磺胺间甲氧嘧啶钠注射液中磺胺间甲氧嘧啶钠和甲氧苄啶的含量。     

HPLC-PDA法同时测定硫酸新霉素可溶性粉中非法添加4种化学药物

建立同时测定硫酸新霉素可溶性粉中非法添加甲硝唑、水杨酸、乙酰甲喹、甲氧苄啶的HPLC-PDA方法。样品用甲醇提取,经C18柱分离,以磷酸盐缓冲液-甲醇为流动相洗脱,流速为1.0 mL/min,采用二极管阵列检测器进行全波长(200～400 nm)扫描,提取波长为230 nm。检查保留时间、峰纯度和光谱相似度,对非法添加化学药物进行确证。结果表明,4种化学药物在0.01～0.12 mg/mL的范围内线性关系良好(r≥0.9998);回收率在98.0％～99.9%之间,RSD≤1.0％,检出限为1～5 g/kg。该检测方法专属性强、操作简便,可用于硫酸新霉素可溶性粉中非法添加4种化学药物的测定。     

五种兽药中非法添加喹乙醇和乙酰甲喹的HPLC-PDA检测方法的建立

建立了高效液相色谱法测定五种制剂中非法添加喹乙醇与乙酰甲喹的方法。以十八烷基键合硅胶为填充剂,乙腈-0.01mol/L磷酸二氢钾(pH 6.0)为流动相,二极管阵列检测器进行全波长(200～400nm)扫描,检测波长为260nm,并采用峰纯度检查和光谱相似度检查辅助对照品比对方法,对非法添加药物进行确证。结果表明,该色谱条件下喹乙醇、乙酰甲喹与其他物质峰分离良好。喹乙醇、乙酰甲喹在0.5～200μg/mL浓度范围内线性良好,回收率在91.1%～105.7%之间,RSD≤3.1%,喹乙醇、乙酰甲喹的检测限分别为1.0mg/g、2.5 mg/g。     

HPLC法测定复方磺胺嘧啶钠注射液的含量

为建立兽药复方磺胺嘧啶钠注射液含量测定的高效液相色谱测定法。采用流动相为0.1%的磷酸溶液-乙腈(85:15,V∶V),色谱柱为C18柱,柱温为40℃,流速为1.0 mL/min,检测波长为240 nm。采用外标法进行定量。磺胺嘧啶钠的线性范围为12.5～200μg/mL,线性方程为Y=44.873X+11.999,r~2=1.000;甲氧苄啶的线性范围为2.5～40μg/mL,线性方程为Y=62.288X+4.0826,r~2=1.000,方法的线性关系良好,添加回收率均大于98%,RSD均小于2%。结果显示该方法简单、精确、可操作,可以用于测量复方磺胺嘧啶钠注射液中磺胺嘧啶钠与甲氧苄啶的含量。     

HPLC-PDA法检测17种兽药中非法添加氨茶碱、二羟丙茶碱的研究

建立了17种兽药中非法添加氨茶碱和二羟丙茶碱的高效液相色谱法,以十八烷基键合硅胶为填充剂,0.025mol/L磷酸二氢钾溶液-甲醇为流动相,二极管阵列检测器全波长(200～400nm)扫描,270nm进行测定,并采用峰纯度检查和光谱相似度检查辅助对照品比对方法,对非法添加药物进行确证。在此液相色谱条件下,氨茶碱和二羟丙茶碱与其他物质峰能很好的分离,两种药物在0.5～200μg/m范围内线性关系良好,相关系数r均为1.0000。按外标法以峰面积计算,氨茶碱和二氢丙茶碱的平均回收率为92.6%～108.3%,RSD为0.05%～3.7%。结果表明,该方法适合兽药中氨茶碱和二羟丙茶碱的检测。     

复方氟苯尼考注射液组分含量测定方法的研究

采用HPLC法,建立复方氟苯尼考注射液中氟苯尼考和甲氧苄啶的含量测定方法。以十八烷基烷键合硅胶为填充剂,乙腈-水-冰醋酸(25∶75∶1)为流动相,检测波长为224 nm,流速1.0 m L/min,进样量为20μL的色谱条件,进行了回收率试验、精密度试验、线性回归试验、干扰试验、耐用性试验。3个浓度氟苯尼考(0.04、0.05、0.06 mg/m L)和甲氧苄啶(0.008、0.01、0.012 mg/m L)的回收率均在98.0%~102.0%,相对偏差RSD值(%)均小于1.50。取含量测定项下的对照品溶液,重复进样6次,以峰面积计算,氟苯尼考和甲氧苄啶的RSD值(%)分别为0.72和0.44,具有良好的重复性。氟苯尼考在0.02~0.08 mg/m L浓度范围内,色谱峰面积与浓度呈良好的线性关系,其回归方程Y=347 555X+698 784(r2=0.999 7);甲氧苄啶在0.008~0.03 mg/m L浓度范围内,色谱峰面积与浓度呈良好的线性关系,其回归方程为Y=472 586X+478 231(r2=1.000 0)。通过改变流动相比例、色谱柱、柱温等色谱条件进行的干扰性和耐用性试验,显示出含量测定结果无明显差异,且系统适应性均符合要求。结果表明:用HPLC方法测定复方氟苯尼考注射液中氟苯尼考和甲氧苄啶的含量,稳定可靠、重现性好、回收率高、结果准确等,可作为该制剂的含量测定方法。     

超高效液相色谱-串联质谱法同时检测鸡蛋中5种磺胺类药物和甲氧苄啶残留量

建立超高效液相色谱-串联质谱法(Ultrahigh-performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定鸡蛋中5种磺胺类药物(磺胺甲恶唑、磺胺二甲嘧啶、磺胺间甲氧嘧啶、磺胺喹噁啉、磺胺二甲氧嘧啶)和甲氧苄啶的残留量的方法。样品经乙腈提取2次, 95%乙腈溶液进行溶解后,过Alumina B Cartridges柱,30%乙腈洗脱,滤膜过滤后滤液用于超高效液相色谱-串联质谱仪测定,外标基质标准曲线法定量。在0.5～100μg/kg的浓度范围内5种磺胺类药物和甲氧苄啶色谱峰面积与浓度呈良好线性相关,相关系数均大于0.99;方法检测限0.5μg/kg、定量限为1.0μg/kg;鸡蛋样品中5种磺胺类药物和甲氧苄啶在1.0～100.0μg/kg添加水平内的平均回收率在66.3%～97.5%之间,批内、批间相对标准偏差在1.4%～11.4%之间。该方法回收率满足残留检测要求,且方法的重现性良好,满足国内外兽药残留相关法规规定。     

高效液相色谱法同时测定复方磺胺间甲氧嘧啶预混剂中磺胺间甲氧嘧啶及甲氧苄啶的含量

建立了同时测定兽药复方磺胺间甲氧嘧啶预混剂中磺胺间甲氧嘧啶及甲氧苄啶含量的高效液相色谱法。以C18柱为固定相,0.1%磷酸溶液－乙腈(86：14)为流动相,流速为1.0mL/min,柱温40℃,检测波长为240nm,采用外标法进行定量。磺胺间甲氧嘧啶的线性范围为5.02~100.36μg/mL,回归方程为Area =0.62 × Amt-0.428 (n=5),r2=0.9996;甲氧苄啶的线性范围为1.01~20.28 μg/mL,回归方程为Area =1.058 × Amt-0.075,r2 = 0.9995。取复方磺胺间甲氧嘧啶预混剂,按磺胺间甲氧嘧啶和甲氧苄啶含量的100%作添加回收实验,分别作8个平行,测得磺胺间甲氧嘧啶的回收率为98.83%~101.95%,RSD为0.91%;甲氧苄啶的回收率为99.02%~103.09%,RSD为1.23%。该方法简单,准确,精密度好,回收率高,可以用于测量复方磺胺间甲氧嘧啶预混剂的含量。     

HPLC-PDA法测定兽药中非法添加的喹乙醇、乙酰甲喹检查方法

建立兽药中非法添加喹乙醇、乙酰甲喹的通用检查方法。以十八烷基键合硅胶为填充剂,0.01 mol/L磷酸二氢钾溶液-乙腈为流动相,梯度洗脱,流速为1.0 mL/min,波长扫描范围为200~400 nm,柱温30℃,采用峰纯度检查和光谱相似度检查辅助对照品比对方法,对非法添加药物进行确证。结果显示,喹乙醇、乙酰甲喹与其他物质峰分离良好;喹乙醇和乙酰甲喹在12种兽药中的平均回收率分别为96.6%~101.4%和98.0%~101.3%,RSD均小于1.4%;喹乙醇和乙酰甲喹的检测限均为1.0 g/kg(L)。该检查方法简便、准确、可靠,可用于检查兽药中非法添加的喹乙醇和乙酰甲喹。     

HPLC法同时测定复方磺胺间甲氧嘧啶钠粉中磺胺间甲氧嘧啶钠和甲氧苄啶的含量

为了建立同时测定复方磺胺间甲氧嘧啶钠粉中磺胺间甲氧嘧啶钠和甲氧苄啶的高效液相色谱方法,试验采用了ECOSIL 120-5-C18（250 mm×4.6 mm,5.0 μm）色谱柱,以乙腈-0.1％磷酸溶液（20：80,V/V）为流动相进行洗脱,流速为1.0 mL/min,检测波长为270 nm,柱温为30℃,进样量为20 μL。结果表明,磺胺间甲氧嘧啶钠和甲氧苄啶色谱峰峰型良好,均能达到完全分离;且在0.5～80 μg/mL范围内线性关系良好（R2>0.999）。精密度和稳定性等考察结果的相对标准偏差（RSD）均小于2.0％;而平均加样回收率均在98％～102％之间,RSD均小于2.0％,均符合方法学要求。采用建立的高效液相色谱法测定了5份供试品中磺胺间甲氧嘧啶钠和甲氧苄啶的含量,结果均符合规定,且与原质量标准方法的测定结果无显著性差异。建立的高效液相色谱法能够用于定量测定磺胺间甲氧嘧啶钠和甲氧苄啶的含量。     

癸氧喹酯干混悬剂含量测定的改进

采用高效液相色谱法测定癸氧喹酯干混悬剂的含量,在2-250μg/mL范围内,峰面积的常用对数与进样量浓度的常用对数呈良好的线性关系,R^2=1(n=5),平均回收率为99.24%~99.51%,RSD在0.05%~0.28%。此方法分析时间短,样品前处理简便、定量结果准确,重现性好,结果满意,为其质量控制提供了依据。     

商会自治的基石——商会自治规范研究

在现代法律秩序中,商会自治规范是制定法的基础和必要的补充,甚至在某些方面替代了制定法;商会自治规范主要包括商会组织规范、行为规范、惩罚规范以及争端解决规范等;其效力仅及于其内部成员;商会自治规范和制定法之间存在冲突,但也存在整合的基础。     

猪毛色遗传的研究进展

本文概述了猪的毛色类型、猪的毛色遗传模式,着重综述了猪毛色基因分子基础的研究进展,指出存在问题并就未来发展方向做了思考。     

中华人民共和国农业部公告 第267号

为贯彻落实《兽药生产质量管理规范》(简称《兽药GMP》),进一步推动兽药GMP实施进程,我部制定了《兽药生产质量管理规范检查验收办法》,现予公告。本公告自2003年6月1日起施行。附件:兽药生产质量管理规范检查验收办法二○○三年四月十日第一章 总则 第一条 为推动《兽药生产质量管理规范》(以下简称兽药GMP)的实施,规范兽药GMP检查验收工作,制定本办法。 第二条 农业部负责全国兽药GMP管理和检查验收工作;负责制修订兽药GMP检查验收管理规定;负责兽药GMP检查员队伍建设和监督管理工作,负责国际兽药贸易中GMP互认工作。 …     

鸡败血支原体垂直传播模式及其阻断方法

以国际标准强毒Ｒ株人工感染非免疫产蛋鸡,定时扑杀,分别从鼻窦、眶下孔、气管、肺、气囊、卵巢和输卵管分离ＭＧ,并收集感染鸡所产蛋分离ＭＧ。结果表明,人工感染４８小时后上、下呼吸道及肺已被全面感染,９６小时气囊已被感染,１２０小时输卵管已能分离到ＭＧ,卵巢始终分离不到ＭＧ。人工感染鸡自１４４小时便能在其所产蛋中分离出ＭＧ。药物治疗能在７２小时内消除感染,油乳剂苗则需２４天后逐渐降低蛋内ＭＧ分离率,药物卵内注射、种蛋药浴、高温处理均能杀死卵内ＭＧ,但以研制的种蛋浸泡剂药浴效果为最好。     

Comparison of 2 methods of centesis of the bursa of the biceps brachii tendon of horses

REASONS FOR PERFORMING STUDY: Centesis of the bicipital bursa using an 8.9 cm long spinal needle has been reported but the alternative of employing a 3.8 cm long hypodermic needle requires validation. OBJECTIVE: To compare the efficacy of 2 different methods of centesis of the bicipital bursa and to evaluate the usefulness of ultrasonographic imaging to determine the location of solution administered when centesis of the bursa is attempted. METHODS: For Trial 1, 6 clinicians, who had no previous experience of centesis of the bicipital bursa, attempted to inject a solution composed of an aqueous radiopaque contrast medium and physiological saline solution (PSS) into the bicipital bursae of 2/12 horses using the previously described distal approach to inject one bursa and a proximal approach to inject the contralateral bursa. The bicipital tendon and bursa were examined ultrasonographically before and after injection; and both shoulders were examined radiographically to identify the location of the medium. In Trial 2, another 6 clinicians, also with no previous experience of centesis, repeated Trial 1, using 6 horses, but the radiopaque contrast medium was mixed with air instead of PSS. RESULTS: Accuracy of centesis using the proximal approach was 39% and that of the distal approach 28%. Ultrasonographic examination of the shoulder allowed the location of solution and air to be accurately predicted in all 12 shoulders examined. CONCLUSIONS: Clinicians who have had no previous experience performing centesis of the bicipital bursa are unlikely to be successful in centesis using either approach. Radiographic examination after injecting a radiopaque contrast medium may be necessary to assess the success of centesis especially if bursal fluid is not obtained during centesis. Injecting air along with the radiopaque contrast medium provides more accurate ultrasonographic confirmation of centesis and better radiographic definition than does injection without air.     

不同样本商品蜂蜜中硒含量的测定

用硝酸和高氯酸消化蜂蜜,使硒游离出来,在微酸性环境下,硒和2,3-二氨基萘(DAN)生成有较强荧光的物质,用环己烷萃取,在激发波长378nm,荧光波长518nm处测定其荧光强度。蜂蜜中硒含量范围:0.10～0.82μg/g。表明:蜂蜜应视为天然富硒营养品。     

乳酸杆菌益生作用机制的研究进展

乳酸杆菌作为益生菌广泛用于人和动物。本文综述了乳酸杆菌改善宿主健康的机制。乳酸杆菌可通过产生抗菌物质如乳酸、过氧化氢、细菌素,或者通过竞争营养或肠道黏附位点来抑制致病菌;通过诱导黏附素的分泌或阻止细胞凋亡而增强肠道的屏障功能,从而保护肠道。文章重点讨论了乳酸杆菌表面成分（表面蛋白、脂磷壁酸和肽聚糖）与肠道受体（Ｃ型凝集素受体、Ｔｏｌｌ样受体和 Ｎｏｄ样受体）,阐述了他们结合后启动免疫调节信号,调控肠道免疫功能以发挥改善健康作用的机制。     

Effects of size of ingestively masticated fragments of plant tissues on kinetics of digestion of NDF

Ingestively masticated fragments were collected and sized via sieving. Different sizes of esophageal masticate and ruminal digesta fragments, and ground fragments of larger masticated pieces were incubated in vitro, and undigested NDF remaining at intervals of up to 168 h of incubation was determined. The ruminal age-dependent time delay (tau) for onset of digestion of NDF was positively correlated (P < 0.004) with the mean sieve aperture estimated to retain 50% of the fragments between successive sieve apertures (MRA). Degradation rate of potentially degradable NDF (PDF) and level of indigestible NDF were not related (P > 0.10) to MRA of masticated and ground fragments. Estimates of tau were positively related to MRA, with slopes of bermudagrass < corn silage < ruminal fragments of corn silage. It was concluded that fragment size-, and consequently, ruminal age-dependent onset of PDF degradation of a mixture of different fragment sizes results in an age-dependent rate of degradation of the more rapidly degrading of two subentities of PDF. Models are proposed that assume a tau before onset of simultaneous degradation of PDF from two pools characterized as having gamma-modeled age-dependency and age-constant rates. The ruminal age-dependent pool seems to be associated with the faster-degrading pool, and its rate parameter increases with range in MRA in the population of fragments. Conceptually, the ruminal age-dependent rate parameter for PDF degradation seems to represent a composite of several effects: 1) effects of the size-dependent tau; 2) range in MRA of the population of ingestively masticated fragments; and 3) subentities of PDF that degrade via more rapid age-dependent rates compared with subentities of PDF that degrade via age-constant rates. The estimated fractional rates of ruminative comminution of ingestively masticated fragments (0.060 to 0.075/h) were of a magnitude similar to the mean fractional rates of PDF digestion (0.030 to 0.085/h), which implies that ruminative comminution may be first-limiting to fractional rate of PDF digestion. The in vivo roles of ingestive and ruminative mastication of fragments on PDF degradation must be considered in any kinetic system for estimating PDF digestion in the rumen. These results and others in the literature suggest that the rate of surface area exposure rather than intrinsic chemical attributes of PDF may be first-limiting to degradation rate of PDF in vivo.