Residue Detection of Tetracyclines in Eggs by High Performance Liquid Chromatography

The study was aimed to establish the method of simultaneous detection of four kinds of tetracyclines,including oxytraoycline,tetracycline,chlortetracycline and doxyeycline in eggs by high performance liquid chromatography (HPLC).The eggs samples were detected with HPLC after through the procedure of extraction of 0.1 mol/L Na₂EDTA-Mcllvaine buffered solution,purification of Oasis MAX solid-phase extraction column,gradient elution of taking acetonitrile-0.01 mol/mL trifluoroacetic acid as mobile phase,separation with reverse liquid chromatography.The results showed that the calibration curves of four kinds of tetracyclines were linear correlated in the concentration range of 30 to 1 000 ng/g which the limits of detection was 10 ng/g and the limit of quantification was 50 ng/g.The average recoveries were 67.3% to 81.4%,relative standard deviations of intraday was 2.7% to 14.3%,relative standard deviations of inter-day was 0.9% to 5.0%.This mothod established in this study could simultaneously detect oxytetracycline,tetracycline,chlortetracycline and doxycycline drug residues in egg and it had high sensitivity,accuracy and precision.The method was rapid and simple to operate.     

HPLC测定宫衣净酊中葛根素含量

为了建立宫衣净酊中葛根素的高效液相色谱(HPLC)测定方法,应用色谱柱为安捷伦Eclipse XDB-C18(4.6mm×250mm,5μm),流动相为甲醇-水(25∶75),流速为1mL/min,检测波长为250nm,柱温为30℃。结果表明,在此色谱条件下,葛根素的线性范围为18.25μg/mL~584.00μg/mL(r=0.999 9,n=6),平均回收率为108.83%(RSD=1.03%)。说明本方法简便、准确、重现性好,可以作为宫衣净酊的质量控制方法。     

Comparative pharmacokinetics of marbofloxacin in healthy and Mannheimia haemolytica infected calves

The pharmacokinetics of marbofloxacin were investigated in healthy (n=8) and Mannheimia haemolytica naturally infected (n=8) Simmental ruminant calves following intravenous (i.v.) and intramuscular (i.m.) administration of 2 mg kg(-1) body weight. The concentration of marbofloxacin in plasma was measured using high performance liquid chromatography with ultraviolet detection. Following i.v. administration of the drug, the elimination half-life (t(1/2 beta)) and mean residence time (MRT) were significantly longer in diseased calves (8.2h; 11.13 h) than in healthy ones (4.6 h; 6.1 h), respectively. The value of total body clearance (CL(B)) was larger in healthy calves (3 ml min(-1) kg(-1)) than in diseased ones (1.3 ml min(-1) kg(-1)). After single intramuscular (i.m.) administration of the drug, the elimination half-life, mean residence time (MRT) and maximum plasma concentration (C(max)) were higher in diseased calves (8.0, 12 h, 2.32 microg ml(-1)) than in healthy ones (4.7, 7.4 h, 1.4 microg ml(-1)), respectively. The plasma concentrations and AUC following administration of the drug by both routes were significantly higher in diseased calves than in healthy ones. Protein binding of Marbofloxacin was not significantly different in healthy and diseased calves. The mean value for MIC of marbofloxacin for M. haemolytica was 0.1+/-0.06 microg ml(-1). The C(max)/MIC and AUC(24)/MIC ratios were significantly higher in diseased calves (13.0-64.4 and 125-618 h) than in healthy calves (8-38.33 and 66.34-328 h). The obtained results for surrogate markers of antimicrobial activity (C(max)/MIC, AUC/MIC and T > or = MIC) indicate the excellent pharmacodynamic characteristics of the drug in diseased calves with M. haemolytica, which can be expected to optimize the clinical efficacy and minimize the development of resistance.     

烷基-二醇基硅胶填料的合成及对莠去净类除草剂的在线分离

三步合成了烷基-二醇基硅胶(ADS)色谱材料，首先用γ-缩水甘油醚氧丙基三甲氧基硅烷把功能基团键合到硅胶基体上，再把该环氧化硅胶与硬脂酸反应以制备酯型十八烷基反相填料，最后在20MPa压力下装成色谱预柱(35×4.6mm I.D)。用该预柱通过六通阀后接ODS分析柱(250×4.6mm I.D)，构成中心切割二维HPLC。该系统能对具有一定疏水性的化合物进行在线富集，实现环境及生物复杂样品直接进样分离分析。使用该系统对尿中的莠去净和西玛津残留进行了分离分析，以含有0.1%乙酸的酸性水缓冲液对加标尿液中莠去净类化合物保留在预柱上，干扰分析的大分子被排阻而无保留通过，其它干扰分子保留小而通过，再切换六通阀，以乙腈和0.1%乙酸水溶液进行梯度洗脱，进而在下一级ODS分析柱上进行分离（紫外检测225nm），两种除草剂的分离分析取得了良好的定性定量结果     

比久和多效唑混合物的高效液相色谱分析

在吸光度为210nm、流动相配比为甲醇：乙腈：水＝40：20：40的条件下，多效唑和比久均能得到很好的分离。比久的保留时间约为3．19min，多效唑的保留时间约为11．83min。加标回收率：比久为108．69％，多效唑为90．39％。     

高效液相法测定普洱茶焙烤制品中儿茶素及咖啡碱含量的研究

为准确测定普洱茶经焙烤后有效物质儿茶素及咖啡碱的保留率,建立了高效液相法,采用70%甲醇提取液提取茶焙烤制品中的儿茶素,并使用C18反相色谱柱,以乙酸乙腈-乙酸水为流动相进行梯度洗脱,流速为1 mL/min;在波长为270 nm下经紫外分光法检测,结果表明:普洱茶粉的有效成分在焙烤过程中的保留率高,其中总儿茶素的平均保留率达90.55%,咖啡碱的平均保留率高达99.46%,因此该检测方法具有简便、准确、分离效果好的优点,适用于检测茶焙烤食品中儿茶素的含量。     

HPLC紫外法同时检测生鲜乳中环丙沙星和恩诺沙星残留

[目的]建立能同时检测环丙沙星和恩诺沙星残留的HPLC紫外检测法。[方法]采用10%三氯乙酸为提取液,直接从生鲜乳中提取环丙沙星和恩诺沙星,并进行HPLC检测。[结果]环丙沙星和恩诺沙星的最低检测限为5μg/L,在10~200μg/L浓度范围内呈良好的线性关系(r0.99),平均回收率为84%~112%,变异系数均小于5%。[结论]该方法不仅除蛋白和脂肪效果好,而且回收率较为理想,可以很好满足确证方法的要求,且重现性好。     

环丙沙星在猪体内的生物利用度及药物动力学

18 头健康长白×大白×杜洛克杂交猪,分3 组,每组6 头,按5 m g/kg 的剂量进行了静注、肌注及内服环丙沙星的药动学研究。高效液相色谱法测定血浆中药物的质量浓度,MCPKP药代动力学程序处理药时数据。静注给药时,环丙沙星体内分布快且广泛,消除较慢,t1/2α为(0.35±0.19) h,t1/2β为(3.15±0.57) h,Vd(area)为(3.24±0.51) L/kg,ClB 为(0.73±0.15) L/(kg·h- 1 )。肌注和内服给药时,环丙沙星均吸收较快,但内服吸收速度和程度均不及肌注给药,t1/2ka 分别为(0.23±0.15)、(0.38±0 .21) h,tm ax 分别为(0.63±0.31)、(1.39±0.39) h,Cm ax 分别为(1.31±0.34)、(0.60±0.14) m g/L,生物利用度(F)分别为(77.96±5.89)% 、(51.58±5.69)% 。本研究发现,环丙沙星肌注和内服给药的消除半衰期与静注给药相似,分别为(3.45±0.66)、(3.32±0.96) h,与在其他哺乳动物的动力学特征有所不同。     

恩诺沙星在猪组织中残留消除规律研究

在常规饲养条件下,对健康猪按2.5 mg/kg体重的剂量肌肉注射2.5%恩诺沙星注射液,每日2次,连续注射3 d.停药后第2、4、6、8、10、12、14天分别屠宰4头猪.分别采取每头猪的肌肉(注射部位)、脂肪(腹脂)、肝和肾脏等4种组织,用高效液相色谱法进行残留量测定.结果表明:残留在肌肉、脂肪组织中的药物消除较快,第8天总残留量(恩诺沙星 环丙沙星)已下降至检测限(20μg/kg)以下;肝和肾脏组织中的药物消除缓慢,第14天测得猪肾中药物总残留量为40μg/kg.     

HPLC法测定盐酸氨丙啉的含量及对杂质2-甲基吡啶进行检查

采用高效液相色谱法测定盐酸氨丙啉的含量及对杂质2-甲基吡啶进行检查.用Waters XTerraTM RP C18色谱柱,以乙腈-甲醇-庚烷磺酸钠溶液(将12 g的1-庚烷磺酸钠溶于1000 mL水中,加24mL冰醋酸,6 mL的三乙胺制得)(5:35:60)为流动相,用紫外检测器于254nm处检测,柱温30℃,流速1.0 mL/min.在该条件下盐酸氨丙啉和2-甲基吡啶的分离度很好,盐酸氨丙啉浓度在0.05～0.50 mg/mL范围内,其色谱峰面积与浓度呈良好的线性关系,回归方程为y=3.07×107x-3.90×104,r=0.999 9,RSD=0.76%.该法适用于盐酸氨丙啉原料药的质量控制.