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建立了饲料中As(Ⅲ)、As(Ⅴ)、氨苯胂酸(p-ASA)和洛克沙胂(ROX)不同形态砷的高效液相色谱-电感耦合等离子体-串联质谱(HPLC-ICP-MS/MS)检测方法。样品经甲醇-水(1∶1,V/V)超声提取,用Shiseido MGⅡC18色谱柱(250×4.6 mm,5μm)对4种砷形态进行分离,以pH=4.7的6mmol/L四丁基氢氧化铵(TBAH)-甲醇(92∶8,V/V)溶液及pH=1.9的0.05%三氟乙酸(TFA)-甲醇(92∶8,V/V)溶液为流动相进行梯度洗脱。然后通过电感耦合等离子体质谱进行监测,外标法定量。结果表明,在优化的实验条件下,各形态砷在0~50μg/L范围内线性良好(R≥0.9999),As(Ⅲ)、As(Ⅴ)、氨苯胂酸(p-ASA)和洛克沙胂(ROX)的检测限分别为0.05、0.10、0.08、0.60μg/L,4种形态砷的加标回收率范围在85.9%~104.6%之间,相对标准偏差(RSD)均小于5%。通过对实际样品的检测,该方法适用于饲料中常见形态砷的检测。 相似文献
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建立了高效液相色谱-电感耦合等离子体串联质谱(HPLC-ICP-MS/MS)同时测定土壤中阿散酸(p-ASA)、洛克沙胂(ROX)及其降解产物无机砷(i-As)(亚砷酸(As(Ⅲ))和砷酸(As(Ⅴ)))、一甲基砷(MMA)和二甲基砷(DMA)等5种砷形态的分析方法。以0.1 mol/L NaH_2PO_4-0.1 mol/L H_3PO_4(体积比9∶1)为提取剂,液固比为50 mL/g,样品经微波辅助提取(80℃,30 min)后,采用Hamilton PRP-X100阴离子交换柱(250 mm×4.1 mm,10μm),以60 mmol/L(NH_4)_2HPO_4-5%甲醇(pH 6.0)和水为流动相进行梯度洗脱,在15 min内实现了5种砷形态的良好分离。在优化条件下,各砷形态在0~500μg/L范围内线性良好(r~2≥0.999 1),检出限为0.043~0.080μg/kg(以As计),相对标准偏差为1.7%~3.8%。将该方法用于分析3种土壤样品,各砷形态的加标回收率为71.6%~106%。该方法简单、快速、准确、可靠,适用于土壤中阿散酸、洛克沙胂和常规砷形态的检测。 相似文献
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建立了饲料中亚砷酸盐(As~(3+))、砷酸盐(As~(5+))、一甲基砷酸(MMA)、二甲基砷酸(DMA)、对氨基苯胂酸(p-ASA)、羟基苯胂酸(4-OH)和洛克沙胂(ROX)共7种不同形态砷的高效液相色谱-氢化物发生原子荧光光谱(HPLC-HG-AFS)分析方法。饲料样品采用甲醇-水(1∶1,V/V)溶液提取,15 mmol/L(NH_4)_2HPO_4和10 mmol/L邻苯二甲酸氢钾为流动相,经PRP-X100阴离子交换色谱柱分离后,由HG-AFS测定。结果表明,7种砷形态标准曲线的线性关系良好(R2≥0.9964),方法检出限为5~30 μg/kg,平均回收率为76.3%~108.1%,日内相对标准偏差≤7.7%,日间相对标准偏差≤17.4%。本方法灵敏度高、前处理简单、运行费用低廉,适用于饲料产品中砷的形态分析。 相似文献
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苏宇亮 《理化检验(化学分册)》2009,45(5)
对高效液相色谱-电感耦合等离子体质谱联用技术在水质分析中的应用作了评述,对高效液相色谱-电感耦合等离子体质谱联用技术的发展前景作了展望.引用文献48篇. 相似文献
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《理化检验(化学分册)》2015,(8)
综述了近年来六价铬的测定方法,包括分光光度法、离子色谱法、高效液相色谱-电感耦合等离子体质谱联用法和离子色谱-电感耦合等离子体质谱联用法的研究进展,并对六价铬测定方法的发展前景进行了展望(引用文献51篇)。 相似文献
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高效液相色谱-电感耦合等离子体质谱联用测定鸡肉及鸡肝中10种砷形态化合物 总被引:1,自引:0,他引:1
建立了一种有效分离检测鸡肉及鸡肝样品中洛克沙砷(ROX)、阿散酸(ASA)、硝苯胂酸(NPAA)、卡巴胂(CBS)、砷酸(AsⅤ)、亚砷酸(AsⅢ)、一甲基胂酸(MMA)、二甲基胂酸(DMA)、砷甜菜碱(As B)和砷胆碱(As C)共10种砷形态化合物的高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)分析方法。采用10%甲醇为提取液,碳酸铵溶液为流动相,以阴离子分析柱将样品提取液进行分离,最后进行ICP-MS测定。10种砷形态化合物在0.1~100μg/L范围内线性关系良好,相关系数(r2)均大于0.999,检出限为0.3~1.5μg/kg,定量下限为1.0~5.0μg/kg,加标回收率为81.3%~97.7%,相对标准偏差为0.1%~3.5%。该法重现性好、灵敏度高,且采用组织研磨仪机械振荡5 min即可成功提取10种砷形态化合物,与常规水浴加热振荡提取相比更加简便、高效。该法适用于鸡肉及鸡肝样品中10种砷形态化合物的同时检测,通过对实际样品的分析测定,在鸡肝样品中检出阿散酸和亚砷酸。 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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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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Jona Mirnik Eva Pušavec Kirar Sebastijan Ričko Uroš Grošelj Amalija Golobič Franc Požgan Bogdan Štefane Jurij Svete 《Tetrahedron》2017,73(24):3329-3337
A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu0 as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than CuI in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT). 相似文献
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George E. Magoulas Thomas Garnelis Constantinos M. Athanassopoulos Dionissios Papaioannou George Mattheolabakis Konstantinos Avgoustakis Dimitra Hadjipavlou-Litina 《Tetrahedron》2012,68(35):7041-7049
(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C60, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine. 相似文献