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1.
建立了动物源食品中喹喔啉类药物代谢残留标识物3-甲基喹喔啉-2-羧酸和喹喔啉-2-羧酸的高效液相色谱-串联质谱检测方法。样品在酸性环境水解,经乙酸乙酯、磷酸盐缓冲液依次提取,Oasis MAX固相萃取小柱净化,用Waters Xterra MS C18柱(150 mm×2.1 mm, 5 μm)分离,以甲醇-0.2%甲酸为流动相梯度洗脱,采用多反应监测(MRM)正离子模式检测,内标法定量。各物质在1.0~20.0 μg/L范围内线性关系良好,相关系数均不低于0.9996; 3-甲基喹喔啉-2-羧酸和喹喔啉-2-羧酸在0.1、0.2、1.0 μg/kg加标水平的回收率为62.4%~118%,相对标准偏差为1.48%~28.1%;定量限(以信噪比≥10计)为0.1 μg/kg。该方法简单、灵敏、稳定,可满足猪肉、猪肝、鸡肉、鸡肝、鱼、虾等动物源食品中3-甲基喹喔啉-2-羧酸和喹喔啉-2-羧酸残留的检测与确证需要。 相似文献
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动物组织中卡巴氧和喹乙醇以及相关代谢产物的液相色谱-串联质谱检测方法 总被引:6,自引:1,他引:5
建立了牛、猪肌肉和肝脏组织中卡巴氧(CBX)和喹乙醇(OQX)以及相关代谢产物--脱氧卡巴氧(DCBX)、喹噁啉-2-羧酸(QCA)和3-甲基喹噁啉-2-羧酸(MQCA)残留的LC-MS/MS的检测方法.组织样品中的卡巴氧用乙腈-乙酸乙酯(体积比1 : 1)溶液提取;代谢产物的提取则是经适当处理后的样品加入Protease蛋白酶进行酶解,后采用阴离子交换固相萃取柱Oasis MAX进行净化和富集.分析样品以甲酸溶液(体积分数为 0.1%)-甲醇-乙腈为流动相,经Inertsil ODS-3色谱柱分离,在LC-MS/MS多反应监测模式下进行定性、定量分析,采用正离子扫描.CBX、DCBX、QCA和MQCA的定量下限均为0.5 μg/kg,猪、牛肌肉和肝脏在0.5 ~5.0 μg/kg添加水平的平均回收率在76% ~97%之间,相对标准偏差(n=10)在2.9% ~16.9%之间. 相似文献
3.
高效液相色谱法测定动物组织中3-甲基喹喔啉-2-羧酸残留量 总被引:5,自引:0,他引:5
本文建立了猪、鸡、鱼肌肉及猪、鸡肝脏组织中喹乙醇代谢残留标识物3-甲基喹喔啉-2-羧酸残留量的高效液相色谱分析方法.样品在酸性环境水解,经乙酸乙酯、磷酸盐缓冲溶液依次提取,Oasis MAX固相萃取柱净化,高效液相色谱紫外测定(HPLC-UV).3-甲基喹喔啉-2-羧酸标准曲线相关系数(r2)为0.9992(10~1 000 μg/L);不同动物组织样品中3-甲基喹喔啉-2-羧酸工作曲线相关系数(r)为0.9995~0.9997(2~100 μg/kg).在2~100 μg/kg浓度范围,3-甲基喹喔啉-2-羧酸回收率为69%~104%,日内相对标准偏差<15%,日间相对标准偏差<20%.检出限(CCα)为1.2~4.3 μg/kg,定量限(CCβ)为2.0~5.6 μg/kg. 相似文献
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用气相色谱-质谱法对乙酰甲喹样品中的共存物进行定性、定量分析,确定样品中含有3种与乙酰甲喹结构类似的化合物,即3-甲基-2-乙酰基喹噁啉、3-甲基-2-乙酰基喹噁啉-4-氧化物、3-甲基-2-乙酰基喹噁啉-1-氧化物,其相对含量分别为4%、20%、30%,乙酰甲喹相对含量为46%。 相似文献
7.
以玻碳电极为工作电极,在pH为6的甲醇-B.R.缓冲溶液的混合溶液中,3,4-二氢-2-羟基喹噁啉在+0.48V有一氧化峰,2-羟基喹噁啉在-0.98V有一还原峰,峰高与相应的电活性物质浓度分别在2.8+10~(-6)—8.0×10~(-5)mol/L和8.0×10~(-6)—6.4×10~(-4)mol/L范围内有良好的线性关系。在此条件下,对样品中二者含量进行了同时测定。 相似文献
8.
建立了牛奶和奶粉中卡巴氧代谢物喹喔啉-2-羧酸(QCA)和喹乙醇代谢物3-甲基喹喔啉-2-羧酸(MQCA)残留量的液相色谱-串联质谱测定方法。将样品经0.6%(体积分数)的甲酸溶液进行消化,用Tris缓冲溶液调节pH后,加入Protease蛋白酶进行酶解,样品溶液用0.3 mol/L HCl溶液酸化后,采用阴离子交换固相萃取柱Oasis MAX进行净化和富集。分析样品以0.1%(体积分数)的甲酸溶液-甲醇-乙腈为流动相,经Inertsil ODS-3色谱柱分离,采用负离子扫描,在LC-MS/MS多反应监测模式下进行定性及定量分析。喹口恶啉-2-羧酸和3-甲基喹口恶啉-2-羧酸的方法测定下限牛奶为0.5μg/kg,奶粉为4.0μg/kg。对牛奶在0.5~5.0μg/kg,奶粉在4.0~40.0μg/kg添加水平的平均回收率为68.2%~82.5%,RSD为3.4%~12%。 相似文献
9.
建立了高效液相色谱-串联质谱同时定量和确证猪肉中3-甲基喹喔啉-2-羧酸(MQCA)残留量的检测方法。试样用0.3 mol/L盐酸溶液水解提取,加入乙腈和乙酸乙酯萃取,再用0.1 mol/L氢氧化钠溶液反萃取,阴离子交换固相萃取柱净化,经Agilent Eclipse Plus C18柱(50 mm×3.0 mm,1.8 μm)分离,采用液相色谱-串联质谱仪检测,基质匹配添加标准曲线定量。MQCA在1.0~50 μg/L范围内线性相关系数大于0.99,在0.5、1.0、5.0 μg/kg加标水平下其回收率为90.5%~119.6%,相对标准偏差为3.14%~4.22%。方法可用于猪肉中MQCA残留量的快速定量和确证检测。 相似文献
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用电子轰击质谱(EI-MS)研究了1-烷基-3-甲基-2(1H)-喹喔啉-2-酮(烷基为H,CH3,Et,n-C5H11),1-烷基-3-甲基-6-硝基-2(1H)-喹喔啉-2-酮(烷基为CH3,Et)和1-甲基-3-甲基-6-胺基-2(1H)-喹喔啉-2-酮,结合其结构特征总结出一些裂解规律。讨论了不同取代基对这类化合物熔点的影响,结果表明:在同类喹喔啉化合物中,随着烷基链的增长,样品熔点通常会有所降低,而硝基及胺基的引入会使其熔点升高。 相似文献
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Syntheses of Boc-protected 4-amino- and 5-amino-pyrrole-2-carboxylic acid methyl esters have been achieved and the structures of these compounds have been fully characterized by detailed NMR studies. 相似文献
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This paper describes the use of potentiometric titration to determine the relevant acid–base properties of 5-hydroxypyrazine-2-carboxylic
acid (5OH-PYCA), an important intermediate in the production of tuberculostatics. The data obtained were used for calculation
of the dissociation constants of 5OH-PYCA. It was found that 5OH-PYCA dissociates in two steps, with the corresponding dissociation
constants pK
a1=3.42 and pK
a2=7.96, designating 5OH-PYCA as a medium weak acid (1st step). The distribution diagram of dissociated species and the buffer-strength
diagram of 5OH-PYCA provide useful information about its behaviour at different pH. The ionic equilibria data obtained can
be used for selection of the optimum pH for biotransformation of pyrazine-2-carboxylic acid (PYCA) and for prediction of pH
changes during the biotransformation. These data can also be used for selection of the optimum pH for precipitating 5OH-PYCA
in downstream processing. All computations have been optimized by mathematical modelling using Solver. 相似文献
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Investigations were made to determine the TLC properties of monosubstituted pyridines. The primary aim was to identify and quantitatively determine the monohydroxypyridines formed during in vitro chemical and enzymatic hydroxylation experiments.TLC studies were carried out not only on the monosubstituted pyridines, but also on 2,3-di-OH-pyridine and 3-OH-pyridine-N-oxide.The UV absorption spectra of pyridine and its substituted derivatives were recorded at a concentration of 10−3 M in ethanol, and were compared.The best TLC detection of these derivatives was elaborated too. 相似文献
2. Rf Values of Monohydroxypyridines and other Monosubstituted Pyridines (Monoamines and Monocarboxylic Acids) in Systems I and II
15.
I. D. Ivanchikova G. É. Usubalieva P. V. Schastnev A. A. Moroz M. S. Shvartsberg 《Russian Chemical Bulletin》1992,41(9):1672-1679
The Cu(I)-catalyzed intramolecular cyclization of 1-phenylethynyl-and 1-hexyn-1-yl-anthraquinone-2-carboxylic acid is a 6-endo-dig-addition, whereas the reaction for 1-(3-phenoxypropyn-1-yl)anthraquinone-2-carboxylic acid proceeds in a directionally nonspecific way. It is shown that the cyclization of vicinal acetylenic derivatives of aromatic carboxylic acids leads to the formation of the more stable of the possible cyclic structures.Institute of Chemical Kinetics and Combustion, Siberian Branch, Russian Academy of Sciences, 630090 Novosibirsk. Novosibirsk State University, 630090 Novosibirsk. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 9, pp. 2138–2146, September, 1992. 相似文献
16.
《Journal of Coordination Chemistry》2012,65(2):335-347
Abstract Mn(II) cations in the crystals of trisaquobis(μ-thiophen-2-carboxylato-O,O′)(thiophen-2-carboxylato-O)manganese(II) monohydrate are bridged by oxygen atoms donated by bidentate carboxylic groups of two thiophen-2-carboxylate ligands. In addition, each Mn(II) ion is coordinated by an oxygen atom of a monodentate carboxylic group of this ligand and three oxygen atoms of water molecules. The coordination around the Mn(II) cation is octahedral. The bridging of the ligands results in molecular ribbons propagating in the c-direction of the crystal held together by C?H…O hydrogen bonds. The crystal structure of diaquobis(μ-furan-3-carboxylato-O,O′)di(μ-furan-3-carboxylato-O,O)(μ-aqua-O)manganese(II) consists of dinuclear structural units. In each molecule Mn(II) cations are O,O′ bridged by oxygen atoms of bidentate carboxylic groups of two furan-3-carboxylate ligands and have a water located between the Mn cations. The units are O,O′ bridged to Mn(II) ions located in adjacent units by bidentate oxygen atoms, forming molecular ribbons extending in the c-direction. Octahedral coordination around each Mn(II) ion is completed by two water molecules. The octahedra around two adjacent metal ions in the unit share a common apex - the bridging oxygen atom of the water molecule. The ribbons are held together by C?H…O hydrogen bonds between furan ring oxygen atoms and the carbon atoms of adjacent furan rings. 相似文献
17.
《Analytical letters》2012,45(5):445-449
Abstract The reagent ethyl cyanoglyoxalate phenyl-2-carboxyllc acid hydrazone has been developed for the selective amperometric determination of thorium. Commonly associated ions like UO2+ 2, Pe3+, La3+, Ce4+, and Zr4+ do not interfere even when present in ten fold molar excess. 23μg to 4.6mg thorium can be determined within an error of ±1.5 percent. 相似文献
18.
A new version of the Friedländer synthesis of 2-aminoquinoline-3-carboxylic acid and its derivatives from stable 2-tosylaminobenzaldehyde or its morpholinal was proposed. 相似文献