超高效液相色谱—串联质谱法检测鸡血液样品中喹诺酮类药物残留     

超高效液相色谱&#x  串联质谱法检测鸡血液样品中喹诺酮类药物残留 《畜牧与饲料科学》2019,40(11):13-16

旨在建立鸡血液样品中多种喹诺酮类药物残留的超高效液相色谱—串联质谱方法。样品经乙腈提取,经Waters Acquity UPLC BEH C₁₈色谱柱分离,以甲醇和0.1%甲酸水溶液为流动相进行梯度洗脱,电喷雾正离子（ESI⁺）模式电离,MRM扫描模式检测。经方法学验证,该方法的线性关系、回收率、精密度均符合要求。应用超高效液相色谱—串联质谱法建立了鸡血液样品中多种喹诺酮类药物同时检测的方法,实现了动物血液样品中12种喹诺酮类药物同时定性、定量分析。  相似文献   

钙在橄榄树器官中的定量研究   总被引：3，自引：0，他引：3  

钟明  甘廉生 《中国南方果树》2004,33(4):21-23

本研究用原子吸收光谱法分析了果园土壤及橄榄树体各器官中钙量和不同组分钙的含量。结果表明：0～30cm土层中钙含量最高为0．65mg／g。橄榄器官中叶的钙含量最高为4．523mg／g，其次为根、果、结果枝。地上部器官钙含量由主干一主枝一结果枝一叶片逐渐增加。在各器官中钙主要以醋酸溶钙和盐酸溶钙的形式存在。  相似文献   

用紫外分光法测定鱼藤中异黄酮类的总含量     

陈欣安  陆磊 《中南林业科技大学学报(自然科学版)》1996,(1)

根据鱼藤中异黄酮类化合物在紫外光２１０～２４５ｎｍ及２９０～３０５ｎｍ处具有吸收峰这一特性，提出了用紫外分光法测定鱼藤中异黄酮类总含量的方法．在３００ｎｍ波长处，浓度低于６×２．６１８×１０－３／ｍｏｌ·Ｌ－１时，测定了标准系列的吸光值，结果表明吸光值与浓度近乎直线相关，相关系数为０．９９７７；标准系列吸光值准确性高；加样回收率达９９％以上；测定样品时，重现性好．  相似文献   

蛋白质组学研究技术及其在果树学中的应用   总被引：7，自引：3，他引：7  

曹尚银  张秋明  郭俊英  陈玉玲 《果树学报》2005,22(2):138-142

蛋白质组研究是当今生命科学发展的一个新的增长点,它能阐明基因组所表达的真正执行生命活动的全 部蛋白质的表达规律和生物功能。简要介绍了蛋白质组学产生的科学背景、研究方法和研究内容。蛋白质组学研究 方法主要有双向聚丙烯酰胺凝胶电泳(2D-PAGE)、质谱(Mass-spectrometric)技术、蛋白质芯片(Protein chips)技术、酵母 双杂交系统(Yeast two-hybrid system)、双向高效柱层析和生物信息学等。其应用的范围包括植物群体遗传学、在个体 水平上植物对生物和非生物环境的适应机制、植物的发育和组织器官的分化过程,以及不同亚细胞结构在生理生态 过程中的作用等诸多方面。同时展望了植物蛋白质组学研究前景以及蛋白质组学技术在果树学中的应用前景。  相似文献   

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   

Histological and proteomics analysis of apple defense responses to the development of Colletotrichum gloeosporioides on leaves     

《Physiological and Molecular Plant Pathology》2015

Colletotrichum gloeosporioides (Penz.) Penz. & Sacc. is an important fungal pathogen known to cause glomerella leaf spot (GLS). The objective of this study was to analyze the infection of C. gloeosporioides on leaves of apple cv. Fuji (resistant) and cv. Gala (susceptible) and apply proteomics techniques to study the apple defense responses 48 h after inoculation (h.a.i.). On both of cultivars, C. gloeosporioides started to germinate at 3 h.a.i. on adaxial surface and produced appressoria adhering to epidermal cell juxtapositions. Histological analysis showed more stratified parenchyma in leaves of cv. Fuji than cv. Gala associated with differences in the chemical composition of cell walls. Total and unique proteins expressed by cvs. Fuji and Gala at 3, 12, 24 and 48 h.a.i. were detected by comparative proteomes analysis. A total of 42 unique proteins expressed at 24 and 48 h.a.i. were identified by MALDI/TOF mass spectrometry, and most of these proteins were identified as directly involved in defense responses.  相似文献   

核磁共振法测定甲哌鎓原药的含量     

魏泱  王晓莉  郭幸丽  刘晶晶 《农药科学与管理》2014,35(12):49-52

采用定量核磁共振法建立了甲哌鎓原药的定量方法。以重水为溶剂,仲丁基脲为内标物,以化学位移分别在δ3.12的甲哌鎓甲基和δ1.10的仲丁基脲甲基的1H-NMR信号作为定量峰。以甲哌鎓与仲丁基脲定量峰的峰面积比(AS/AI)对甲哌鎓与仲丁基脲的质量比(WS/WI)进行线性回归,线性相关系数为0.999 9;重复测定同一批次原药含量,变异系数为0.28%。采用核磁共振波谱法对甲哌鎓进行定量分析,操作简便,测定速度快,准确度高。  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   

磷酸、膦酸酯类农药的质谱裂解规律研究     

李娇 《农药科学与管理》2016,(6):25-30

在对23种磷酸、膦酸酯类农药及其氧化物的质谱数据进行归纳整理的基础上,明确了这类农药质谱裂解规律。结果表明:电子轰击离子化条件下,磷酸、膦酸酯类农药分子极易裂解,且分子离子峰较弱。发现C_2H_6O_3P~+(m/z109)是其最具代表性的特征碎片离子。磷酸酯类农药裂解规律是二甲氧基磷酸酯P-0键易发生a断裂,生成m/z 109特征碎片离子。二乙氧基磷酸酯易脱去中性碎片C_2H_4,形成m/z81的特征离子。R'含有烯烃结构,易产生m/z127的特征碎片离子。膦酸酯类农药裂解规律与磷酸酯类似,特征性弱,膦键容易发生a断裂。选定了磷酸、膦酸酯类农药在质谱分析中常见的碎片离子,为农药残留筛查、确证分析提供参考。  相似文献