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为建立测定盐酸氯苯胍原料药中主成分含量及有关物质的超高效液相色谱法,采用ACQUITY UPLC BEH C18柱(1.7μm,2.1mm×100mm),以乙腈-2mL/L磷酸水(V∶V=40∶60)为流动相,检测波长为313nm,进样量10μL。在优化的色谱条件下,主成分与各杂质峰分离度良好,盐酸氯苯胍在15μg/mL~35μg/mL范围内线性关系良好(R2=0.999),低、中、高浓度样品的平均回收率分别为100.85%、100.61%、100.40%,相对标准偏差(RSD)分别为1.50%、0.07%、0.64%。盐酸氯苯胍的主要杂质为保留时间1.612的R1和5.416的R2,以主成分自身对照法计算,暂定单个杂质峰面积不得大于对照溶液主峰面积的0.16倍(0.16%),各杂质峰面积的和不得大于对照溶液主峰面积的0.26倍(0.26%)。该方法分离时间短,检出限低,分离度好,结果准确、可靠,可作为盐酸氯苯胍及其有关物质的检测方法。 相似文献
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《中国畜牧兽医》2020,(6)
为快速有效地检测动物源性食品中氯苯胍及其代谢物残留,研究建立一种在鸡蛋、鸡肉、牛肉、鱼肉和猪肉5种动物源性食品中,同时检测氯苯胍及其代谢物(对氯苯甲酸、对氯苯甲酰氨基乙酸)残留的超高效液相色谱-串联质谱(UPLC-MS/MS)法。样品经过2%(V/V)甲酸乙腈溶液提取,无水硫酸钠去除水分,氮吹浓缩后甲醇复溶,正己烷除脂,高速冷冻离心,得到净化后的样品进行上机测定。选用Waters ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7μm),将甲醇—0.1%甲酸水溶液作为流动相进行梯度洗脱。通过多反应检测(MRM),在正/负离子模式下,采用基质匹配外标法,同时对3种化合物进行定性和定量分析。结果显示,氯苯胍、对氯苯甲酸和对氯苯甲酰氨基乙酸在各自浓度范围内线性关系良好,相关系数R~20.999。氯苯胍的检出限(LOD)和定量限(LOQ)分别为0.5和1.0μg/kg,对氯苯甲酸的LOD和LOQ分别为2.5和5.0μg/kg,对氯苯甲酰氨基乙酸的LOD和LOQ分别为1.0和2.5μg/kg。不同基质中,3种化合物在4个添加水平(氯苯胍:1.0、25、50、100μg/kg;对氯苯甲酸:5.0、25、50、100μg/kg;对氯苯甲酰氨基乙酸:2.5、25、50、100μg/kg)的平均回收率为76.0%~95.9%,相对标准偏差(RSDs,n=6)为2.6%~10.6%。基质效应|ME|为0.2%~26.2%,其中氯苯胍在鸡蛋中,对氯苯甲酰氨基乙酸在鸡肉、牛肉和鱼肉中存在较强的基质效应(|ME|20%),空白猪肉可作为代表基质用于3种化合物的定量分析。本方法前处理简单,灵敏度较高,重现性好,可用于动物源食品中氯苯胍及其代谢物残留的测定。 相似文献
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为快速有效地检测动物源性食品中氯苯胍及其代谢物残留,研究建立一种在鸡蛋、鸡肉、牛肉、鱼肉和猪肉5种动物源性食品中,同时检测氯苯胍及其代谢物(对氯苯甲酸、对氯苯甲酰氨基乙酸)残留的超高效液相色谱-串联质谱(UPLC-MS/MS)法。样品经过2%(V/V)甲酸乙腈溶液提取,无水硫酸钠去除水分,氮吹浓缩后甲醇复溶,正己烷除脂,高速冷冻离心,得到净化后的样品进行上机测定。选用Waters ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7 μm),将甲醇-0.1%甲酸水溶液作为流动相进行梯度洗脱。通过多反应检测(MRM),在正/负离子模式下,采用基质匹配外标法,同时对3种化合物进行定性和定量分析。结果显示,氯苯胍、对氯苯甲酸和对氯苯甲酰氨基乙酸在各自浓度范围内线性关系良好,相关系数R2>0.999。氯苯胍的检出限(LOD)和定量限(LOQ)分别为0.5和1.0 μg/kg,对氯苯甲酸的LOD和LOQ分别为2.5和5.0 μg/kg,对氯苯甲酰氨基乙酸的LOD和LOQ分别为1.0和2.5 μg/kg。不同基质中,3种化合物在4个添加水平(氯苯胍:1.0、25、50、100 μg/kg;对氯苯甲酸:5.0、25、50、100 μg/kg;对氯苯甲酰氨基乙酸:2.5、25、50、100 μg/kg)的平均回收率为76.0%~95.9%,相对标准偏差(RSDs,n=6)为2.6%~10.6%。基质效应|ME|为0.2%~26.2%,其中氯苯胍在鸡蛋中,对氯苯甲酰氨基乙酸在鸡肉、牛肉和鱼肉中存在较强的基质效应(|ME|>20%),空白猪肉可作为代表基质用于3种化合物的定量分析。本方法前处理简单,灵敏度较高,重现性好,可用于动物源食品中氯苯胍及其代谢物残留的测定。 相似文献
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HPLC-MS/MS法同时测定水产品中的诺氟沙星、盐酸小檗碱、盐酸氯苯胍残留 总被引:1,自引:0,他引:1
建立了一种同时测定水产品中诺氟沙星、盐酸小檗碱和盐酸氯苯胍残留量的HPLC-MS/MS法。样品经1%甲酸甲醇提取,正己烷脱脂,冷冻、离心后,用高效液相色谱-串联质谱仪,选择反应监测(SRM)、正离子模式进行定性和定量分析。结果表明:诺氟沙星、盐酸小檗碱和盐酸氯苯胍在1~100 ng/mL范围内线性关系良好,线性相关系数≥0.9996,检出限为1 ng/g。诺氟沙星、盐酸小檗碱、盐酸氯苯胍在5、50和100 ng/g三个添加水平下,三种水产品肌肉的平均加标回收率在79.83%~104.06%之间,相对标准偏差在2.97%~9.15%之间。本方法重现性好,灵敏度高,能够满足水产品中诺氟沙星、盐酸小檗碱和盐酸氯苯胍的残留检测和药代动力学的研究需要。 相似文献
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<正> 猪食盐中毒时检查胃内容物中氯的含量对于确诊有很大价值(健康猪胃内容中氯的含量在0.31%以下)。为进行食糜的氯化物定量,可用1/10N的硝酸汞溶液滴定,但因硝酸汞货源少,作者试用硝酸银滴定胃容物中氯化物含量,取得满意效果,其原理为胃内容物浸出滤液中氯化物被硝酸银沉淀为氯化很,以铬酸钾为指示剂,使多余之硝酸银作用成为砖红色的 相似文献
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超高效液相色谱-串联质谱法测定鸡组织中氯苯胍残留 总被引:2,自引:1,他引:1
研究建立了鸡组织中氯苯胍残留的超高效液相色谱-串联质谱检测方法。样品经酸化乙腈提取后,分别经中性氧化铝柱和HLB固相萃取柱净化,C18柱分离,超高效液相色谱-串联质谱测定,外标法定量。氯苯胍在10 ng/mL~500 ng/mL的浓度范围内呈线性相关,相关系数为0.994以上。本方法对氯苯胍在鸡组织中的检测限为5μg/kg,定量限为10μg/kg;鸡肉、鸡肝和鸡肾在添加50μg/kg~200μg/kg浓度范围内,其回收率为76.7%~107.6%,鸡脂肪和鸡皮在添加100μg/kg~400μg/kg浓度范围内, 其回收率为81.2%~106.8%, 批内变异系数均在1.4%~19.5%之间,批间变异系数在2.5%~12.8%之间。本方法快速、灵敏、重现性好,各项技术指标均满足国内外相关法规要求,适用于鸡组织中氯苯胍的残留检测。 相似文献
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饲料中盐酸氯苯胍的测定 总被引:2,自引:0,他引:2
盐酸氯苯胍(Robenidine hydrochloride)化学名称为1,3-双[(对氯苯叉)氨基]胍盐酸盐。盐酸氯苯胍是一种高效的抗球虫药,毒性小,疗效高,且适口性好,对鸡、兔的急性、慢性球虫病均有较好效果。然而,使用不当会使肉蛋产品产生异味,如有报道证明,在肉鸡日粮中添加量为66g/t时,屠宰的新鲜肉质中就会有异味,以33g/t的含量饲喂蛋鸡时,在鸡蛋中就会察出异味。为此,农业部2001年第168号公告“饲料药物添加剂使用规范”中规定,饲料中添加10%盐酸氯苯胍预混 相似文献
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魏静 《四川畜牧兽医学院学报》2009,(4):28-32
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。 相似文献
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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。 相似文献
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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。 相似文献
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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. 相似文献
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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. 相似文献