UHPLC-Q/TOF MS结合HPLC-DAD定性和定量分析硫酸黏菌素可溶性粉中的未知添加物     

陆春波  包爱情  周芷锦  张航俊  陈慧华 《中国兽药杂志》2018,52(12):54-60

定性和定量分析一批兽药硫酸黏菌素可溶性粉中的未知添加物。照《中国兽药典》2010年版一部对该批检品用微生物检定法进行含量测定时,发现该样品的抑菌圈为虚圈,用薄层色谱鉴别该样品,未显示与标准品溶液一致的主斑点,怀疑该样品中有处方外非法添加物。采用超高效液相色谱-四级杆-飞行时间质谱(UHPLC-Q/TOF MS)对该样品进行筛查,发现疑似添加物,并使用液相色谱-二极管阵列检测(HPLC-DAD)法进行了双重确证和含量测定。该样品中非法添加物确证为磺胺氯达嗪和甲氧苄啶,添加量分别为58.5 mg/g和13.4 mg/g。本研究通过建立筛查方法为监管部门提供技术支撑,通过分析非法添加物的可能原因为打击兽药处方外非法添加提供了思路。  相似文献   

Pharmacokinetics of articaine hydrochloride and its metabolite articainic acid after subcutaneous administration in red deer (Cervus elaphus)     

D Venkatachalam  JP Chambers  K Kongara  P Singh 《New Zealand veterinary journal》2018,66(1):16-20

AIM: To develop and validate a simple and sensitive method using liquid chromatography-mass spectrometry (LC-MS) for quantification of articaine, and its major metabolite articainic acid, in plasma of red deer (Cervus elaphus), and to investigate the pharmacokinetics of articaine hydrochloride and articainic acid in red deer following S/C administration of articaine hydrochloride as a complete ring block around the antler pedicle.

METHODS: The LC-MS method was validated by determining linearity, sensitivity, recovery, carry-over and repeatability. Articaine hydrochloride (40?mg/mL) was administered S/C to six healthy male red deer, at a dose of 1?mL/cm of pedicle circumference, as a complete ring block around the base of each antler. Blood samples were collected at various times over the following 12 hours. Concentrations in plasma of articaine and articainic acid were quantified using the validated LC-MS method. Pharmacokinetic parameters of articaine and articainic acid were estimated using non-compartmental analysis.

RESULTS: Calibration curves were linear for both articaine and articainic acid. The limits of quantifications for articaine and articainic acid were 5 and 10?ng/mL, respectively. Extraction recoveries were >72% for articaine and >68% for articainic acid. After S/C administration as a ring block around the base of each antler, mean maximum concentrations in plasma (C_max) of articaine were 1,013.9 (SD 510.1) ng/mL, detected at 0.17 (SD 0.00) hours, and the C_max for articainic acid was 762.6 (SD 95.4) ng/mL at 0.50 (SD 0.00) hours. The elimination half-lives of articaine hydrochloride and articainic acid were 1.12 (SD 0.17) and 0.90 (SD 0.07) hours, respectively.

CONCLUSIONS AND CLINICAL RELEVANCE: The LC-MS method used for the quantification of articaine and its metabolite articainic acid in the plasma of red deer was simple, accurate and sensitive. Articaine hydrochloride was rapidly absorbed, hydrolysed to its inactive metabolite articainic acid, and eliminated following S/C administration as a ring block in red deer. These favourable pharmacokinetic properties suggest that articaine hydrochloride should be tested for efficacy as a local anaesthetic in red deer for removal of velvet antlers. Further studies to evaluate the safety and residues of articaine hydrochloride and articainic acid are required before articaine can be recommended for use as a local anaesthetic for this purpose.  相似文献   

Effect of L-lysine Added in Diluent on the Fresh Semen Quality of Dorper Sheep     

MAO Ran  LI Qing-quan  SHI Yan  LAN Xiang-li  WANG Min  ZONG Ze-jun  XIA Guo-zhong  HAN Tian-long 《中国畜牧兽医》2015,42(12):3308-3314

In order to explore the effect of different L-lysine levels added in semen dilution on the fresh Dorper sheep quality stored at liquid state,3 health Dorper ram were used to collect semen which were equal-packaged and added to solution containing different levels (0,0.1,0.2,0.3,0.4 and 0.5 g) L-lysine in 120 mL diluent and at 0,6,24,30,48,54,72 and 78 h,the sperm motility,membrane integrity and acrosome integrity were detected.The results showed that the sperm motility in groups added 0,0.1 and 0.2 g L-lysine were higher than other groups,and that in 0.4 and 0.5 g L-lysine groups decreased faster than other groups;The sperm motility in 0.5 g L-lysine group reduced to 0 at 30 h,and it reduced to 0 at 48 h in the group added 0.4 g L-lysine;The effective survival time and survival index in the group added 0.1 g L-lysine was higher than other groups (P< 0.05);The membrane integrity of 0.1 g group was the highest,that had no significant difference with control group from 0 to 54 h (P >0.05),while after 72 h the two groups had significant differences (P< 0.05).The membrane integrity in 0.4 and 0.5 g groups were the worst,and that was significant different with other groups (P< 0.05);The acrosome integrity of 0.1 g group was the highest which had no significant difference with control group (P >0.05),0.4 and 0.5 g groups were the worst,the difference between them was not significant (P >0.05),while was extremely significant difference with other groups except for 0 and 6 h (P< 0.01).The results suggested that dilution added a high concentration of L-lysine could inhibit sperm quality,when the count of L-lysine was more than 0.2 g,sperm quality was significantly decreased,adding 0.1 g L-lysine could improve Dorper sheep fresh sperm quality stored at liquid state.  相似文献   

兴安藜芦提取液对榆紫叶甲幼虫的防治效果     

常江春  邵红  纪艳  房月春  岳旭  单晓晶  罗志文 《安徽农业科学》2015,(34):180-181

[目的]明确野生兴安藜芦对榆紫叶甲不同龄期幼虫的防治作用.[方法]以野生兴安藜芦为材料,采用70％乙醇、60％丙酮、沸水对藜芦的根、茎、叶分别进行提取,研究各提取液对榆紫叶甲2龄、3龄、4龄幼虫的防治效果.[结果]兴安藜芦不同药用部位的杀虫活性具有明显差异,以根提取物的杀虫活性最强,叶提取物的杀虫效果最差;不同提取方法的杀虫效果也有明显不同,以70％乙醇提取液的杀虫活性最强.[结论]试验结果为榆紫叶甲的生物防治提供了参考.  相似文献   

基于霍尔效应的微小压强测量装置的设计与实现     

占宏  乔利国 《湖南农业大学学报(自然科学版)》2015,(1):51-54

针对化工液体的微小压强测量中所存在的测量复杂、精度低的问题，设计一种基于霍尔效应的测量流体微小压强变化的装置。该测量装置通过前端受力装置来承受液体压强的变化而产生一定的位移，并转换成霍尔电动势，经放大调理电路，最后接电压表显示相应的电压值。根据输出电压与液体压强之间的关系即可得到相应深度的压强大小。在实验中，电压表精确到1mV，最小可测量到0.792Pa的压强变化，其测量精度较高。该装置体积小、通用性强，具有较好的应用前景。  相似文献   

固相萃取-高效液相色谱串联质谱法测定油菜薹中反式维生素K1含量     

徐月清  汪丹丹  杨瑞楠  戚欣  马飞  王秀嫔  张奇  张良晓  李培武 《中国油料作物学报》2019,41(6):842

为准确测定反式维生素K1的含量，建立了基于固相萃取-高效液相色谱串联质谱的甘蓝型油菜（Brassica napus L.）菜薹反式维生素K1高灵敏检测技术。样品经正己烷提取、中性氧化铝柱净化后，用C30反相色谱柱，以甲醇 （含0.025%甲酸+2.5 mmol/L甲酸铵）为流动相，采用选择反应监测（selected reaction monitoring, SRM）模式进行定量分析，20 min内可实现顺反异构体色谱分离。方法学考察结果显示，反式维生素K1在范围内线性关系良好，相关系数为0.9985。该方法检出限为0.29 μg/kg，定量限为0.95 μg/kg。回收率为87.5%～117.6%，精密度（RSD）在0.72% ～9.59%之间。利用该方法对油菜薹和反式维生素K1含量高的3种蔬菜进行分析，发现油菜薹中反式维生素K1含量为340.08 μg/100g，高于小白菜（B. rapa spp. chinensis，260.93 μg/100g）、西兰花（B. oleracea var. Italic Planch， 167.65 μg/100g）和结球甘蓝（B. oleracea var. capitata，151.11 μg/100g）。本文建立的蔬菜中反式维生素K1准确定量分析方法操作简单、灵敏度高、结果准确。同时比较发现油菜薹是一种富含维生素K1的蔬菜。   相似文献   

菜籽油裂解燃料离子液体催化酯化反应降酸工艺的研究     

张爱华  李洋  肖志红  张良波  皮兵  李昌珠 《湖南林业科技》2014,(5):47-49

为了降低裂解燃料酸值,增加燃料的稳定性能,将吡啶丁烷磺酸硫酸氢盐应用于菜籽油裂解燃料的酯化反应。考察了催化剂用量、反应时间和反应温度等对酸值的影响,并在最佳优化条件下考察了裂解燃料成品的理化性质。结果表明:吡啶丁烷磺酸硫酸氢盐对催化酯化反应具有很高的催化活性。优化工艺条件为:催化剂用量1.2%、反应温度75℃、反应时间70 min,在此工艺条件下,酸值降低到1.0 mgKOH/g以下。  相似文献   

液态奶生产新设备和工艺     

郭瑞雪  郭俭 《中国乳业》2021,(12):137-140

液态奶包括巴氏杀菌奶、UHT超高温灭菌奶等。目前国内采用的液态奶杀菌工艺是热处理法。但通过热处理法的液态奶仍可能残留休眠芽孢,给液态奶产品带来潜在风险。本文通过研究目前液态奶杀菌工艺的种类和存在问题,申报了发明专利“一种能延长液态奶保质期的生产方法”和“一种能使液体隔离空气的无菌罐体”,并利用氢医学制作含氢乳制品,实现了提高液态奶品质,延长保质期,获得氢分子医学效应。  相似文献   

超高效液相色谱串联质谱法对水产品中硝基呋喃代谢物的测定     

王狄  张嘉楠 《河北渔业》2016,(7):47-51

建立了使用Waters UPLC Xevo TQ超高效液相色谱串联质谱仪检测水产品中4种硝基呋喃代谢物的分析方法。匀浆后的样品在酸性环境下水解,并用2-硝基苯甲醛衍生16h,经磷酸氢二钾提取,LMS固相萃取小柱净化后,在三重四极杆多反应监测模式下进行测定。方法采用同位素内标法定量,四种代谢物的检出限(LOD)均低于0.25μg·kg-1,线性范围在0.5μg·L~(-1)到10μg·L~(-1)间,相关系数大于0.99。在0.5、1.0和5μg·kg-1浓度下分别进行添加回收试验(n=5),回收率在75.2%~123.3%之间,相对标准偏差(RSD)小于9.4%。  相似文献   

An improved method for extraction of sorghum polymeric protein complexes     

《Journal of Cereal Science》2020

A method for fractionating sorghum proteins using extraction solvents and techniques designed to obtain polymeric protein structures (especially disulfide linked) was developed. Extraction and separation conditions were optimized in terms of completeness of protein extraction, sample stability, and analytical resolution. After pre-extraction of albumins and globulins, a 3-step sequential procedure involving no reducing agents was applied to ground whole sorghum flour. The three fractions obtained represented proportionally different protein polymer contents and molecular weight distribution as evidenced by comparative size exclusion chromatography. Protein composition also varied among the extracts with differences in kafirin composition and non-kafirin proteins detected in the fractions by RP-HPLC and SDS-PAGE analysis. The ability to quantify and further characterize sorghum polymeric protein complexes will be useful for additional studies linking protein structures with functionality and digestibility and variations for these properties within diverse sorghum germplasm.  相似文献