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猪食用组织中喹喔啉-2-羧酸的高效液相色谱检测方法 总被引：6，自引：0，他引：6
为了监测猪食用组织中卡巴氧(carbadox)的残留,建立了检测猪肝脏、肾脏、肌肉等组织中卡巴氧的标示残留物喹喔啉2羧酸(Quinoxaline-2-carboxylic acid,QCA)的高效液相色谱法.组织样品经碱水解,液液分配提取,用离子交换色谱柱净化,洗脱液作浓缩后用甲醇溶解进行测定.色谱柱为ODS C18柱;流动相为甲醇-水(体积比4060),每1L中加入8 mL冰乙酸,流速为1.0 mL/min;定量分析用紫外检测器,波长320 rm,确证性分析用二极管阵列检测器,波长250～500 nm.喹喔啉-2-羧酸工作液质量浓度在0.03～0.96 mg/L范围内,药物峰面积与浓度呈良好的线性关系,相关系数r=0.999 9.组织中添加药物的质量分数为0.015、0.03、0.06 μg/g时,肝脏样品回收率分别为(73.55士9.46)%、(80.33±14.95)%、(75.84±7.42)%;肾脏样品分别为(70.89±10.33)%、(74.89±7.19)%、(83.33±10.68)%;肌肉样品分别为(69.49±7.26)%、(66.44±5.09)%、(62.11±6.08)%.本方法条件下,3种组织中药物最低检出质量分数均为0.015 μg/g,回收率测定的日内及日间相对偏差(RSD)分别＜18%和＜20%.当组织中药物质量分数达0.06μg/g时,可检测到喹喔啉-2-羧酸的特征性紫外吸收光谱. 相似文献
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为检测猪、鸡可食性组织中喹噁啉类兽药残留标示物喹噁啉-2-羧酸(QCA)和3-甲基喹噁啉-2-羧酸(MQ-CA),建立了同时检测这2种残留标示物的高效液相色谱-串联质谱法.将样品碱水解,乙酸乙酯等液-液萃取,65℃氮气吹干,甲醇:0.5%甲酸水溶液(30:70)溶解,0.45μm微孔滤膜过滤后,采用高效液相色谱-串联质谱分析.结果显示,猪、鸡可食性组织中喹噁啉类兽药残留标示物MQCA和QCA检测限为0.2～0034μg/kg和0.5～0.9μg/kg,定量限为0.5～0.61μg/kg和0.77～1.31μg/kg.相对回收率在90.07%～106.8%范围内,日内变异系数≤13.69%.日间变异系数≤15.43%.MQCA和QCA在2～100μg/kg范围内具有较好的线性关系(r~2>0.99).结果表明,本方法简单、灵敏度高.适用于猪、鸡可食性组织中喹噁啉类兽药残留标示物的定量检测. 相似文献
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高效液相色谱法测定中兽药制剂中喹噁啉类药物 总被引：4，自引：2，他引：2
建立了中兽药制剂中喹乙醇、乙酰甲喹、卡巴氧、喹烯酮等药物含量测定的高效液相色谱法。样品经三氯甲烷∶甲醇(3∶1)提取后,苯基柱分离,在360 nm处检测。四种喹噁啉类药物在0.2~100μg/mL浓度范围内呈线性相关。在空白样品中添加50~150 mg/kg,回收率范围在87.90%~96.82%之间,批内变异系数为0.55%~4.65%。本方法的检测限为20 mg/kg,定量限为50 mg/kg。结果表明,本方法适合中兽药制剂中喹噁啉类药物的测定。 相似文献
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《中国兽医学报》2010,(1)
为检测猪、鸡可食性组织中喹噁啉类兽药残留标示物喹噁啉-2-羧酸(QCA)和3-甲基喹噁啉-2-羧酸(MQ-CA),建立了同时检测这2种残留标示物的高效液相色谱-串联质谱法。将样品碱水解,乙酸乙酯等液-液萃取,65℃氮气吹干,甲醇∶0.5%甲酸水溶液(30∶70)溶解,0.45μm微孔滤膜过滤后,采用高效液相色谱-串联质谱分析。结果显示,猪、鸡可食性组织中喹噁啉类兽药残留标示物MQCA和QCA检测限为0.2~0.34μg/kg和0.5~0.9μg/kg,定量限为0.5~0.61μg/kg和0.77~1.31μg/kg。相对回收率在90.07%~106.8%范围内,日内变异系数≤13.69%,日间变异系数≤15.43%。MQCA和QCA在2~100μg/kg范围内具有较好的线性关系(r20.99)。结果表明,本方法简单、灵敏度高,适用于猪、鸡可食性组织中喹噁啉类兽药残留标示物的定量检测。 相似文献
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《饲料研究》2015,(11)
建立超高效液相色谱-串联质谱(LC-MS/MS)联用技术同时测定全价饲料中喹烯酮、喹乙醇、乙酰甲喹、卡巴氧和喹赛多等5种喹噁啉类药物的分析方法。样品通过乙腈-乙酸乙酯(1∶1,体积∶体积)溶液提取,Bond Elut Plexa固相萃取柱净化后上机测定。在正离子模式下通过2对离子对进行定性定量分析。结果表明:5种药物在2~100 ng/m L线性关系良好,相关系数均大于0.99,空白饲料在3个添加质量浓度下的平均回收率为65.8%~109.8%,相对标准偏差均小于12%,方法的检测限为5μg/kg,定量限为10μg/kg。该方法适用于饲料中5种喹噁啉类药物的同时测定。 相似文献
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建立了超高效液相色谱法测定氟喹诺酮类药物粉剂中非法添加喹乙醇、乙酰甲喹、卡巴氧及喹烯酮的方法。采用purospher RP-18色谱柱(2.1 mm×100 mm,粒径2.0μm)分离四种喹噁啉类药物,以磷酸溶液和甲醇-乙腈(7.5∶7.0)为流动相进行梯度洗脱,流速0.3 m L/min,二极管阵列检测器检测,采集波长范围为200~400 nm,分辨率为1.2 nm,记录光谱图和365 nm波长处的色谱图。结果显示,四种喹噁啉类药物的浓度在0.2~100μg/m L范围内的线性良好,相关系数r均为0.9999,回收率在98.0%~100.2%范围内,RSD在0.27%~0.89%之间,检测限200 mg/kg。本方法快速、准确,可用于氟喹诺酮类粉剂中非法添加喹噁啉类药物的定性和定量检测。 相似文献
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《国外畜牧学(猪与禽)》2015,(8)
建立鸡肉中喹乙醇代谢标识物3-甲基喹恶啉-2-羧酸(MQCA)的高效液相色谱-串联四级杆质谱(UPLC-MS/MS)残留分析方法。样本在一定温度下酶解、盐酸酸化后,用酸乙酯提取,吹干浓缩后再用0.1%甲酸水溶液+乙腈(V∶V=1∶9)溶解,加入正已烷除杂;以0.1%甲酸水溶液-乙腈为流动相,经C18柱分离,采用多反应监测(MRM)正离子模式进行检测。实验结果表明,MQCA提取效果好,检出限为0.05μg/kg,在0.5μg/kg~5.0μg/kg添加水平的平均回收率在73.72%~95.22%之间,相对标准偏差为1.27%~2.79%。本方法适用于鸡肉组织中喹乙醇代谢物残留检测。 相似文献
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通过贝鲁特反应和还原、脱羧反应在体外合成制备3-甲基喹噁啉-2-羧酸,并进行理化鉴定和抗菌活性测试;通过MTT方法研究3-甲基喹噁啉-2-羧酸对多种细胞的生长抑制作用,利用单细胞电泳研究其对细胞DNA的损伤作用,利用流式细胞术研究其对细胞周期的改变。结果显示,体外成功合成制备出3-甲基喹噁啉-2-羧酸,而3-甲基喹噁啉-2-羧酸几乎没有抗菌效果,对多种细胞的生长抑制作用较弱,在剂量检测范围内细胞抑制率不到30%,但在一定剂量下能导致细胞DNA损伤,主要表现为尾长和尾部DNA含量显著升高;并且3-甲基喹噁啉-2-羧酸也能改变Chang细胞的细胞周期,表现为S期阻滞。结果表明,3-甲基喹噁啉-2-羧酸具有一定的细胞毒性。 相似文献
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Concentrations of carbadox and a first metabolite, desoxycarbadox, were measured in contents of the porcine gastrointestinal tract after in-feed administration of carbadox in therapeutic dosages (100-150 ppm). The levels of carbadox in the relevant parts of the gastrointestinal tract were found to be lower than the MIC-values reported for enteropathogenic microorganisms at their sites of action. The presented observations do not provide a pharmacological rationale for the therapeutic use of carbadox in the treatment of dysentery and diarrhoea in swine. The carbadox levels encountered in the proximal part of the gut (stomach, duodenum) however, seem to indicate that in-feed administration of 50 ppm carbadox can provide an effective prophylaxis against Treponema hyodysenteriae, a causative agent in swine dysentery. The timecourse of the blood levels of carbadox and desoxycarbadox after in-feed administration of carbadox (50 ppm) and the concentration profiles in the gastrointestinal tract are discussed with regard to the disposition of this drug in pigs. 相似文献
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In a growth experiment with 144 pigs of the landrace breed in the body weight range of 20 to 100 kg the effect of Carbadox at constant and decreasing levels in the feed until 60 kg body weight on the growth performance and the digestibility of the nutrients in rations with a varying protein supply was studied. The following results were obtained: The supplementation of Carbadox to protein rich diets caused only a small increase in daily body weight gain and feed conversion ratio. The increase of growth performance as a consequence of the addition of Carbadox was more pronounced with the low protein diets. From this result a protein sparing effect of Carbadox can be derived. The effect of Carbadox on growth performance could be observed from 20 to 60 kg body weight and over the whole experimental period from 20 to 90 kg. The increase of growth performance could be largely explained by a better digestibility of the nutrients. 相似文献
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S B Power W J Donnelly J G McLaughlin M C Walsh M F Dromey 《The Veterinary record》1989,124(14):367-370
A weaner ration containing carbadox at concentrations of 331 to 363 mg/kg was accidentally fed to suckling and weaned pigs in an 84 sow herd. Discarded ration was fed to 36 sows. One hundred and sixty five weaner pigs died in a 10 week period with clinical signs including refusal to eat, ill thrift, the passing of hard pelleted faeces, posterior paresis and death in seven to nine days. The surviving weaners did not thrive and some males showed poor testicular development. Sows and suckling pigs that consumed the ration also failed to thrive as did the progeny of affected sows. The main pathological finding was obliteration of the zona glomerulosa of the adrenal cortex. Increased potassium and decreased sodium concentrations in serum were the most notable and consistent biochemical findings. 相似文献
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G W Thrasher J E Shively C E Askelson W E Babcock R R Chalquest 《Journal of animal science》1969,28(2):208-215
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A 2 X 2 factorial arrangement with two levels (0, 660 ppm) of vitamin C and two levels (0, 55 ppm) of carbadox supplementation was used in two experiments with 112 crossbred pigs weaned between 4 and 5 wk of age. An 18% protein corn-soybean meal-oats-dried whey starter diet was used as the basal diet. Each diet was fed ad libitum for a 4-wk period to three replicates of four pigs in Exp. 1 and to four replicates of four pigs in Exp. 2. Vitamin C supplementation produced a significantly higher plasma vitamin C concentration in weanling pigs, but, contrary to results of our previous study, failed to improve average daily gain of the pigs. Daily gain was, however, improved significantly by carbadox supplementation. Carbadox also produced a significantly higher plasma vitamin C concentration in pigs after a 7-d lag period. Plasma Fe concentration of pigs was not affected by supplemental vitamin C, but was significantly higher in those fed carbadox-supplemented diets. Plasma ceruloplasmin concentration increased significantly in all treatment groups from the initial sampling period (d 0) to subsequent periods. No interactions between supplemental vitamin C and carbadox were observed in daily gain, feed efficiency and the measured plasma constituents. 相似文献
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E J van der Molen J H van Lieshout M J Nabuurs F H Derkx A P Lamers A M Michelakis 《Research in veterinary science》1989,46(3):401-405
Carbadox is known to induce toxic effects on the adrenal cortex, resulting in hypoaldosteronism. To study the involvement of carbadox on the renin-angiotensin system, weaned piglets of five weeks old received feed supplemented with 0 (control group), 50, 100, 150 or 200 ppm carbadox. After four weeks the 100 and 150 ppm groups had significantly higher plasma renin activity levels than the control group and after nine weeks plasma renin activity levels of all treated groups were significantly higher than the control group. Five and 10 weeks after carbadox administration, three and two pigs, respectively, of all groups were necropsied and the kidneys were screened for immunohistochemically demonstrated renin. All dosed pigs demonstrated an increase of immunoreactive renin, which was dose- and time-related. From these results it is concluded that carbadox induces activation of the renin-angiotensin system, secondary to the suppressing effect on mineralocorticoid secretion and that these changes may be responsible for part of the clinical picture. 相似文献
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Leroy G. Biehl Manford E. Mansfield Arnold R. Smith George T. Woods Richard C. Meyer 《Preventive veterinary medicine》1985,3(5):489-497
Purchased feeder pigs from 12 farms were commingled and divided into three treatment groups of carbadox, lincomycin and controls. Health and performance evaluations included serology, bacterial isolations, fecal examinations and post-mortem examinations at slaughter, weight gain, and feed efficiency.Serological tests for influenza, Aujeszky's disease and Mycoplasma hyopneumoniae were negative throughout the study. Bordetella bronchiseptica was isolated from 14% of the pigs on arrival and from 42% of the pigs 30 days after commingling. No Salmonella spp. were isolated from fecal swabs on arrival; Salmonella typhimurium was isolated from 2.5% of the pigs on Day 30, but no Salmonella was isolated on Day 90. Fecal examination on arrival revealed that 12.5% were infected with gastrointestinal parasites (5.0% Trichuris suis, 5.0% Ascaris suum and 2.5% Strongyloides ransomi).During the 30-day treatment period immediately following purchase and commingling, carbadox and lincomycin improved growth rate by 7.6% and 10.2%, respectively. The treatments also improved feed efficiency, by 9.9% and 5.7%, respectively, and uniformity of growth. Growth rate and feed efficiency were not affected by treatment from Days 30 to 90 following removal of the feed additives from the diet.Growth rate varied greatly, depending on the farm of origin. Although the reasons for the differences in performance were not well established, results suggested that transmission of B. bronchiseptica between pigs resulted in decreased growth rate following infection. Carbadox was significantly more effective than lincomycin in preventing transmission of B. bronchiseptica between commingled pigs.Post-mortem examination at slaughter revealed turbinate atrophy in 5.8% of the noses and pneumonia in 18% of the lungs. One liver exhibited evidence of ascarid larval migration. Treatments produced no significant effect (P>0.05) on post-mortem examination results. 相似文献