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芹菜、草莓基质对甲胺磷等4种有机磷农药测定的影响 总被引:1,自引:0,他引:1
研究芹菜、草莓基质对甲胺磷、乙酰甲胺磷、氧化乐果、毒死蜱4种有机磷农药检测的影响。利用样品基质溶液配制标准样品,对比草莓、芹菜样品、丙酮溶液中4种农药的保留时间、峰形、峰面积。结果发现DB–5MS色谱柱上,丙酮溶液、芹菜基质、草莓基质中甲胺磷、乙酰甲胺磷、氧化乐果色谱峰出峰时间不完全重合,保留时间最大漂移0.1 min。丙酮溶剂、芹菜基质较草莓基质中的甲胺磷、乙酰甲胺磷、氧化乐果更容易出现峰拖尾现象,且芹菜基质溶液中相同浓度的甲胺磷、乙酰甲胺磷峰面积分别约是草莓基质溶液中的75%,90%。毒死蜱的保留时间、峰形、响应面积在草莓基质、芹菜基质、丙酮溶液中基本一样。 相似文献
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高效液相色谱-串联质谱法测定烟草中有机磷农药的残留量 总被引:26,自引:1,他引:25
建立了一种基于液相色谱-串联质谱法(LC-MS/MS)定量分析微量有机磷农药残留的方法,并应用于烟草中农药残留物的定量检测。采用乙腈超声提取烟草中的有机磷农药残留,以甲醇-水(含0.1%乙酸铵)(体积比为95∶5)为流动相,经高效液相色谱分离,以串联质谱在多反应监测(MRM)模式下测定,在2.5 min内完成了甲胺磷、乙酰甲胺磷、乐果、敌百虫、毒死蜱5种常用有机磷农药的定量分析。5种农药在1~200 μg/L内的线性关系良好(r>0.998),平均回收率为77%~104%,检出限为1.0~5.0 μg/kg。 相似文献
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液相色谱-串联质谱法测定水产品中7种有机磷类农药残留物 总被引:1,自引:0,他引:1
使用高效液相色谱-串联质谱仪(LC-MS/MS)同时测定水产品中的敌百虫(Dipterex)、敌敌畏(Dichlorvos)、蝇毒磷(Coumaphos)、乙酰甲胺磷(Acephote)、甲胺磷(Methamidophos)、毒死蜱(Chlorpyrifos)、乐果(Dimethoate)等7种有机磷类药物的残留量.采用酸化的乙酸乙酯提取均质后的样品,提取液过酸性氧化铝柱净化去脂,经(LC/MS/MS)电喷雾电离(ESI)源,正离子多反应检测(MRM)模式检测,外标法定量.敌百虫、敌敌畏、蝇毒磷、乙酰甲胺磷、甲胺磷、毒死蜱、乐果检出限均可达到10 μg/kg,在添加浓度10~200 μg/kg之间线性关系良好,相关系数(r)均>0.9990,对于10、15、20 μg/kg水平添加回收率范围在72.9%~106%之间,相对标准偏差(RSDs)范围在1.89%~11.6%之间. 相似文献
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茶叶中乙酰甲胺磷及甲胺磷对映体的气相色谱法分离与测定 总被引:2,自引:0,他引:2
建立了乙酰甲胺磷、甲胺磷对映体在茶叶基质中的手性拆分与定量方法。比较了2种手性柱对乙酰甲胺磷及甲胺磷对映体的分离效果,并对分离效果较优的BGB-176手性柱进行色谱条件优化。茶叶样品经改良QuEChERS法处理后,气相色谱测定,外标法定量。在0.04,0.08,0.4 mg/kg 3个加标水平下,甲胺磷、乙酰甲胺磷的回收率分别为58.3%~66.4%和50.8%~57.6%,相对标准偏差(n=5)均小于7%。方法检出限为0.003~0.01 mg/kg。该方法简便、可靠,满足分析要求。通过实际样品的检测,发现乙酰甲胺磷、甲胺磷对映体在茶树上存在一定的降解差异。 相似文献
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《分析科学学报》2021,37(5)
本文以CdSe/ZnS量子点为荧光探针,基于乙酰甲胺磷对CdSe/ZnS量子点的荧光猝灭效应,建立了一种可快速测定乙酰甲胺磷的荧光检测方法。通过透射电子显微镜(TEM)、紫外-可见吸收光谱和荧光光谱对CdSe/ZnS量子点进行表征。在反应时间为5 min条件下,乙酰甲胺磷的浓度在0.487×10~(-6)~7.225×10~(-6) mol/L范围内与CdSe/ZnS量子点的荧光猝灭强度比值呈良好的线性关系(R~2=0.9987),方法检出限为2.55×10~(-7) mol/L。在2.0、5.0μmol/L加标水平下的回收率为94.5%~102.8%,相对标准偏差(RSD,n=5)小于4%。该方法选择性好,灵敏度高,可用于水果和蔬菜中农药乙酰甲胺磷的快速检测。 相似文献
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构建了以大肠杆菌为指示生物的全细胞微生物传感器,初步探讨了其在重金属(Cu2+,Zn2+,Pb2+)及其二元联合毒物、农药污染物(莠灭净、乙酰甲胺磷)的急性生物毒性分析中的应用性能。结果表明,基于对数生长后期和稳定期的大肠杆菌微生物传感器具有良好的毒性分析性能。最优实验条件为:E.coli培养16 h,苯醌为电子传递介体,呼吸基质pH 6~8。所测毒物对E.coli的呼吸抑制作用大小顺序为:Cu2+>Zn2+>Pb2+,乙酰甲胺磷>莠灭净,与发光细菌、鱼类、藻类等其它方法检测所得结果一致。这种电化学全细胞生物传感器毒性分析方法具有快速灵敏、成本低廉、操作简单等优点,有望用于水体急性生物毒性的在线监测。 相似文献
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Uroš Grošelj Mojca Žorž Amalija Golobič Branko Stanovnik Jurij Svete 《Tetrahedron》2013,69(52):11092-11108
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives. 相似文献
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The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion. 相似文献
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N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%). 相似文献
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Shashikant U. Dighe Surya K. Samanta Shivalinga Kolle Sanjay Batra 《Tetrahedron》2017,73(17):2455-2467
An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y1 and Y2. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones. 相似文献
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In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates. 相似文献
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An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions. 相似文献
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Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described. 相似文献
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用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在. 相似文献
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An efficient tandem approach for the selective synthesis of 4,5-dihydroimidazo[1,5-a]quinoxalines 6a–g and imidazo[1,5-a]quinoxalines 7a–h by the reaction of 2-imidazolyl anilines 4a–c with aryl aldehydes 5a–k under mild reaction conditions is described. Introduction of electron releasing alkyl groups in substrates 4a–b was found to be instrumental for the success of the reaction. 相似文献
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The Diels-Alder reactivity of 1,2-heteroborines (H4C4B(H)X, X?=?NH, PH, AsH; O, S, Se) has been computationally explored by means of Density Functional Theory (DFT) calculations. The influence of the HB?=?X fragment on the reactivity of the system has been quantitatively analyzed in detail by means of the so-called Activation Strain Model (ASM) of reactivity. It is found that the interaction between these species and the dienophile is significantly stronger than that computed for their all-carbon isoelectronic counterpart, benzene. In addition, the strain energy plays a key role in the observed reactivity trends. The role of the aromaticity strength of these heteroarenes on the reactivity is also assessed. 相似文献