HPLC法测定复方防己口服液中粉防己碱和防己诺林碱的含量

为了用HPLC法同时测定复方防己口服液中粉防己碱和防己诺林碱的含量.采用Diamonsil C 18柱(5μm,4.6 mm×250 mm),以乙腈-0.2％磷酸水溶液-三乙胺(63∶37∶0.05)为流动相,流速为1.0 mL/min,检测波长282 nm的液相检测方法.结果表明,在此色谱条件下,粉防己碱和防己诺林碱的分离良好,分别在20.52 ～ 205.2μg/mL和17.84 ～ 178.4 μg/mL浓度范围内峰面积与浓度呈良好的线性关系.按外标法以峰面积计算进行测定,粉防已碱和防己诺林碱的平均回收率分别为98.15％和97.35％,RSD分别为1.39％和1.90％.表明该方法简便,快速,准确,适用于防已散中粉防己碱和防己诺林碱的含量测定.     

高效液相色谱法测定替加氟血药浓度

目的:建立一种高效、准确、快捷的人体血浆中替加氟浓度检测方法。方法:色谱柱:Pronaos EP-C18柱;流动相:甲醇-乙腈-水(10∶5∶85);流速:1.0 mL/min;进样量20μL;柱温25℃;检测波长:λ=270 nm。结果:本法在替加氟浓度(X)为0.415~166μg/mL(r=0.999 9)内线性关系良好。低、中、高3种不同浓度(8.3μg/mL、41.5μg/mL、207.5μg/mL)相对回收率分别为99.64%、97.78%、99.41%,日内、日间精密度的RSD均小于5%。结论:此法用血量少,血浆处理方法简单,具有专一性,适用于临床替加氟血药浓度的监测。     

紫外分光光度法测定甲基丁香酚含量方法的建立

采用紫外分光光度法,检测波长230 nm对甲基丁香酚原料药含量进行测定.结果表明,在Oμg/mL～5 μg/mL浓度范围内线性关系良好,回归方程为A=0.025 1x-0.001 4(r=0.996 6,n=5),平均回收率为99.45％,RSD为1.03％(n=3),测定的甲基丁香酚原料药的含量为98.27％.该方法...     

兽用白头翁颗粒中盐酸小檗碱含量测定方法的建立

采用ZORBAX.SB-C18(4.6 mm×150 mm,5μm)为色谱柱,柱温30℃,流动相为乙腈-0.05 moL/L磷酸二氢钾溶液(50∶50)(每100 mL中加十二烷基硫酸钠0.4 g,以磷酸调节pH值为4),流速为1.0 mL/min,检测波长342 nm,进样量10μL。结果显示:盐酸小檗碱在0.1².5 mg/mL范围内呈良好的线性关系(r=0.999 95,n=7),平均含量为6.23 mg/g,平均加样回收率99.33%(n=9,RSD=0.82%),盐酸小檗碱的定量限为1.0 ng/mL,检测限为0.15 ng/mL。本方法简便、快速、准确、重现性好,可用于兽用白头翁颗粒中盐酸小檗碱的含量测定。     

高效液相色谱法测定饲料中的违禁药物氯丙嗪

试验制定了氯丙嗪的在饲料中残留的HPLC检测方法。高效液相色谱条件为分析柱C_(18)反相色谱柱(250×4.6mm,5μm),流动相为35mmol/L NH_4Ac∶乙晴=35∶65,按0.05％的比例加入三乙胺,流速:2.0mL/min,紫外检测波长:257nm。实验表明,氯丙嗪在0.05～5.00μg/mL的范围内线性良好(r=0.99996)。经过对饲料添加0.50、1.00、2.50μg/g3个浓度,证明此提取条件的回收率在80％以上。该方法快速简便,灵敏度高。最低检测限为0.05μg/mL。     

犬血浆中塞拉菌素含量的高效液相色谱-荧光检测方法的建立

本研究以多拉菌素为内标,建立了犬血浆中塞拉菌素的高效液相色谱-荧光检测方法.用乙腈作为血浆蛋白沉淀剂,用SampliQ C18型SPE固相萃取柱进行净化,用1-甲基咪唑和三氟乙酸酐衍生化处理.色谱条件为ODS-1色谱柱(250 mm×4.6 mm),流动相为甲醇∶乙腈∶1％1-庚烷磺酸∶0.4％乙酸=40.0∶57.6∶0.9 ∶ 1.5(v/v/v/v),流速1mL·min-,进样量20μL,激发波长355 nm,发射波长465 nm,柱温30℃.方法的检测限为0.25 ng·mL-1,线性范围0.5～50.0 ng·mL-,变异系数为1.47 ％～3.31％,方法的样品平均回收率为94.0％.结果表明,所建方法准确、灵敏度高和重复性好,可用于犬体内塞拉菌素血药含量的测定.     

液相色谱-串联质谱法测定禽粪便中尼卡巴嗪的残留量

本试验建立了一种测定禽粪便中尼卡巴嗪(以DNC计)的残留量的超高效液相色谱串联质谱(UPLC-MS/MS)检测方法.以甲醇:0.2％甲酸水溶液(75+25)为流动相,0.2 mL/min流速,30℃柱温下,超高效液相色谱分离,三重串联四级杆质谱多反应监测(MRM)扫描模式检测,DNC-D8同位素内标法进行定量.试验结果表明,DNC浓度在10～1000 ng/mL时,呈良好的线性关系,R2为0.9996;4组不同浓度各6个平行样的回收实验,回收率范围为84.8％ ～ 91.2％,平均回收率达到87.9％;相对标准偏差RSD范围为2.47％ ～ 5.45％.本方法特异性强、定性准确、灵敏度高,完全能满足禽粪便中尼卡巴嗪的残留检测.     

高效液相色谱法同时测定博落回注射液中血根碱和白屈菜红碱的含量

建立了高效液相色谱法测定博落回注射液中血根碱和白屈菜红碱含量的方法。采用Agilent 1260型高效液相色谱仪,配二极管阵列检测器(PDA),色谱柱为waters SymmetryC18(4.6mm×250mm,5μm),柱温:35℃,流速为:1.0mL/min,流动相:乙腈-三乙胺溶液=25∶75(磷酸调pH值至2.5),检测波长270nm。结果表明:血根碱在0.5~100μg/mL范围内线性关系良好(R^2=1.000),平均回收率(n=6)为98.21%,RSD为1.76%;白屈菜红碱在0.25~50μg/mL范围内线性关系良好(R^2=1.000),平均回收率(n=5)为98.77%,RSD为0.83%。本方法简便快捷,可用于博落回注射液中血根碱和白屈菜红碱的含量测定。     

二氢血根碱和二氢白屈菜红碱在鸡肌肉中的定量检测方法

建立了一种用于同时测定鸡肌肉中二氢血根碱和二氢白屈菜红碱的UPLC-MS/MS方法。肌肉样品经乙腈-水(95∶5)溶液超声提取后,离心取上清液经脱脂后氮吹浓缩,甲醇复溶。采用Agilent Poroshell 120 EC-C18(2.1mm×150mm i.d.,2.7μm)色谱柱分离,采用正离子化模式下的多反应监测模式进行测定。方法的特异性良好,二氢血根碱和二氢白屈菜红碱在0.2~200μg/L质量浓度范围内线性关系良好(r2≥0.999 6),最低定量限均为0.4μg/kg,平均回收率分别为103.44%和104.36%,准确度RE均≤10.49%,精密度RSD均≤7.43%。该方法应用于长期饲喂博落回散的健康雌性白羽肉鸡的鸡胸肌组织中二氢血根碱和二氢白屈菜红碱的残留量检测,在500mg/kg博落回散组测得DHSA残留量为0.804μg/kg。该方法灵敏度高,重复性好,适用于鸡肌肉中二氢血根碱和二氢白屈菜红碱的残留定量检测。     

高效液相色谱法同时测定预混剂中盐酸环丙沙星和盐酸小檗碱含量

以C18为固定相,0.002 5 mol/L磷酸溶液(用三乙胺调pH值至3.0±0.1)-乙睛(75∶25)为流动相,335 nm为检测波长,采用高效液相色谱法同时测定盐酸环丙沙星、盐酸小檗碱预混剂中盐酸环丙沙星和盐酸小檗碱的含量。盐酸环丙沙星和盐酸小檗碱线性范围分别为1～600μg/mL和0.4～400μg/mL,平均加标回收率分别为100.0%和100.1%,RSD均为0.11%(n=5)。     

Comparisons of Angus, Charolais, Galloway, Hereford, Longhorn, Nellore, Piedmontese, Salers, and Shorthorn breeds for weight, weight adjusted for condition score, height, and condition score of cows

Breed differences for weight (CW), height (CH), and condition score (CS) were estimated from records (n = 12,188) of 2- to 6-yr-old cows (n = 744) from Cycle IV of the U.S. Meat Animal Research Center's Germplasm Evaluation (GPE) Program. Cows were produced from mating Angus and Hereford dams to Angus, Hereford, Charolais, Shorthorn, Galloway, Longhorn, Nellore, Piedmontese, and Salers sires. Samples of Angus and Hereford sires were 1) reference sires born from 1962 through 1970 and 2) 1980s sires born in 1980 through 1987. The mixed model included cow age, season of measurement and their interactions, year of birth, pregnancy-lactation code (PL), and breedgroup as fixed effects for CW and CS. Analyses of weight adjusted for condition score included CS as a linear covariate. The model for CH excluded PL. Random effects were additive genetic and permanent environmental effects associated with the cow. Differences among breed groups were significant (P < 0.05) for all traits and were maintained through maturity with few interchanges in ranking. The order of F1 cows for weight was as follows: Charolais (506 to 635 kg for different ages), Shorthorn and Salers, reciprocal Hereford-Angus (HA) with 1980s sires, Nellore, HA with reference sires, Galloway, Piedmontese, and Longhorn (412 to 525 kg for different ages). Order for height was as follows: Nellore (136 to 140 cm), Charolais, Shorthorn, Salers, HA with 1980s sires, Piedmontese, Longhorn, Galloway and HA with reference sires (126 to 128 cm). Hereford and Angus cows with reference sires were generally lighter than those with 1980s sires. In general, breed differences for height followed those for weight except that F1 Nellore cows were tallest, which may in part be due to Bos taurus-Bos indicus heterosis for size.     

Supplementation of broodmares with copper, zinc, iron, manganese, cobalt, iodine, and selenium

In experiment 1, 6 pregnant mares received a concentrate that contained a trace mineral premix that provided 14.3 mg Cu, 40 mg Zn, 28 mg Fe, 28 mg Mn, 0.08 mg Co, 0.16 mg I, and 0.16 mg Se/kg concentrate (group A). Seven mares received the same concentrate plus 502 mg Zn and 127 mg Cu once daily (group B). No differences (P > .05) in foal growth data, or Cu, Zn, and Fe concentrations of mare milk, mare serum, or foal serum were observed. In experiment 2, 6 pregnant mares received the same concentrate as group A (group C), and 8 mares received the same concentrate fortified with 4× the trace mineral premix (group D). Group C mares had higher serum Zn concentration at 1 day (P < 0.01) and 56 days (P < 0.04). Group C mares had higher milk Fe concentration at 28 days (P < .01), and group D mares had higher milk Cu concentration at 56 days (P < .01). Group C foals had higher serum Cu concentration at 14 days (P < .03). The results from this study provide no evidence to indicate that supplementing late gestating and lactating mares with higher dietary trace mineral levels than those recommended currently by NRC has any influence on foal growth and development, or on the Cu, Zn, and Fe concentrations of the mare milk, mare serum, or foal serum.     

Concentrations of strontium,barium, cadmium,copper, zinc,manganese, chromium,antimony, selenium,and lead in the liver and kidneys of dogs according to age,gender, and the occurrence of chronic kidney disease

This study was conducted to measure the concentrations of strontium (Sr), barium (Ba), cadmium (Cd), copper (Cu), zinc (Zn), manganese (Mn), chromium (Cr), antimony (Sb), selenium (Se), and lead (Pb) in canine liver, renal cortex, and renal medulla, and the association of these concentrations with age, gender, and occurrence of chronic kidney disease (CKD). Tissues from 50 dogs were analyzed using inductively coupled plasma mass spectrometry. Cu, Zn, and Mn levels were highest in the liver followed by the renal cortex and renal medulla. The highest Sr, Cd, and Se concentrations were measured in the renal cortex while lower levels were found in the renal medulla and liver. Female dogs had higher tissue concentrations of Sr (liver and renal medulla), Cd (liver), Zn (liver and renal cortex), Cr (liver, renal cortex, and renal medulla), and Pb (liver) than male animals. Except for Mn and Sb, age-dependent variations were observed for all element concentrations in the canine tissues. Hepatic Cd and Cr concentrations were higher in dogs with CKD. In conclusion, the present results provide new knowledge about the storage of specific elements in canine liver and kidneys, and can be considered important reference data for diagnostic methods and further investigations.     

电感耦合等离子-质谱法测定饲料中钠、镁、铬、锰、铁、铜、锌、砷、硒、镉和铅

应用电感耦合等离子-质谱技术(ICP-MS),建立饲料中钠、镁、铬、锰、铁、铜、锌、砷、硒、镉和铅等元素的测定方法。对饲料样品的前处理方法、仪器工作参数和11种元素标准曲线进行优化;并以加标回收、分析方法比对和重复测试说明方法的准确性和精密性。方法在0～1 000 ng/ml范围内线性良好,仪器检出限为0.557 7～5.072 ng/ml,具有良好的精密度,其回收率在88.1%～104.4%之间,相对标准偏差小于5.0%。同时与原子吸收和原子荧光方法进行比对,测定结果相近。所建立的方法简单、快速,可替代原子吸收和原子荧光方法测定饲料中的11种金属元素,为饲料的质量控制提供理想的元素分析方法。     

Granulocyte isolation from whole blood of goat, sheep, cattle, horse, dog, pig, and man

A simple two step procedure for the isolation of caprine, ovine, bovine, equine, canine, porcine and human peripheral blood granulocytes is described. After enrichment of granulocytes by centrifugation, contaminating erythrocytes are lysed hypotonically. Recovery, purity, and viability of the granulocyte suspensions are determined. FACScan analysis of the cell suspensions measuring cellular size by forward and sideward light scatter is compared with the corresponding analysis of whole blood leukocytes. Constituencies of the isolated cell suspensions and loss of granulocyte subpopulations through isolation procedure is discussed with regard to granulocyte function assays.     

Department of Clinical Veterinary Practices, School of Veterinary Medicine, University of Dublin, Trinity College, Ballsbridge, Dublin 4

Circular excised skin wounds in the thoracic and metatarsal regions of the dog were studied. A similar sequence of events took place in the two regions although differences did occur due to the different reactions of the tissues which surrounded the wounds. None of the wound cavities became filled with exudate during the early stages of healing. In the thoracic wounds the cavities were largely filled by the swelling and inward movement of adipose tissue. Epithelium first grew on the wound surface in the sector of the wound that was situated in the direction of hair flow. The average time to complete epithelization was similar in both sets of wounds. A zone of alopecia developed around the wounds.     

Effects of butorphanol, flunixin, levorphanol, morphine, and xylazine in ponies

The analgesic and behavioral effects of butorphanol (0.22 mg/kg), flunixin (2.2 mg/kg), levorphanol (0.033 mg/kg), morphine (0.66 mg/kg), and xylazine (2.2 mg/kg), given IM were observed in 8 ponies. These ponies were instrumented to measure response objectively to painful superficial and visceral stimuli. Effects on the cardiopulmonary system and rectal temperature also were evaluated in 6 of these ponies. Observations were conducted before drug injection (base-line values) and after injection at 30, 60, 120, 180, and 240 minutes. Xylazine provided the highest pain threshold for the first 60 minutes and a sedative effect for 105 minutes. The effects for superficial pain and visceral pain persisted 3 hours and 4 hours, respectively. Morphine produced good analgesia for superficial pain (30 minutes), whereas butorphanol provided good effect for visceral pain (4 hours). A slight degree of analgesia for visceral pain was obtained after morphine (1 hour) and levorphanol (4 hours); flunixin did not induce analgesia. Butorphanol, levorphanol, and morphine stimulated motor activity. Behavioral effects did not occur after flunixin was given. Xylazine decreased systolic, diastolic, and mean blood pressures. Marked increases in these pressures, heart rate, and respiratory rate were observed after morphine was given. Changes of central venous pressure, rectal temperature, and blood gas values remained within base-line limits after both drugs were given. Butorphanol increased heart rates for 1 hour; flunixin and levorphanol did not alter any of the above values.