气相色谱-质谱法测定酒中23种邻苯二甲酸酯残留量

应用气相色谱-质谱法测定酒中23种邻苯二甲酸酯残留量。样品在沸水浴中加热除去乙醇后用正己烷提取。离心分离后上清液经DB-5MS石英毛细管色谱柱分离,在选择离子检测模式下进行质谱测定。23种邻苯二甲酸酯的质量浓度均在0.1~10mg·L-1范围内与其峰面积呈线性关系,方法的测定下限(10S/N)为0.5mg·kg-1(DINP及DIDP)和0.1mg·kg-1(其余21种邻苯二甲酸酯)。以空白样品为基体进行加标回收试验,所得回收率在84.1%~100%之间。     

固相萃取-气相色谱-质谱法测定化妆品中20种邻苯二甲酸酯

提出了同时测定化妆品中20种邻苯二甲酸酯类化合物的固相萃取(SPE)-气相色谱-质谱法(GC-MS)。不含油脂和含油脂的化妆品样品分别以正己烷和乙腈为溶剂作超声固相萃取,使其所含邻苯二甲酸酯类化合物溶于有机相中。萃取液经Cleanert PAE30006-C柱净化,所得净化后溶液进行气相色谱-质谱(GC-MS)分析。质谱分析中采用电子轰击正离子模式(EI+)和选择离子监测(SIM)模式,用外标法定量。20种邻苯二甲酸脂类化合物的质量浓度在0.1~10mg·L~(-1)范围内与峰面积呈线性关系,检出限(3S/N)在0.13~1.04 mg·kg~(-1)之间,样品加标回收率在79.2%~123%之间,相对标准偏差(n=6)在1.7%~12%之间。     

气相色谱-串联质谱法同时测定烟用水基胶中15种邻苯二甲酸酯类化合物

采用气相色谱-串联质谱法同时测定烟用水基胶中15种邻苯二甲酸酯类化合物的含量。烟用水基胶样品0.300g经2mL水分散,用10mL正己烷萃取5min。在气相色谱分离中用DB-35MS色谱柱为固定相,在质谱分析中采用多反应监测模式。15种邻苯二甲酸酯类化合物的质量浓度均在0.05~5.0 mg·L~(-1)内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为0.006~0.027μg·g~(-1)。在4,20,100μg·g~(-1)等3个浓度水平进行加标回收试验,回收率为87.8%~104%,测定值的相对标准偏差(n=6)为1.3%~6.1%。     

气相色谱-质谱法测定酒中16种邻苯二甲酸酯

应用气相色谱-质谱法测定酒中16种邻苯二甲酸酯的含量。样品经乙酸乙酯提取,所得提取液用DB-5MS UI色谱柱分离,在全扫描/选择离子监测共用模式下测定。16种邻苯二甲酸酯的质量浓度均在0.5~10.0mg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.01~0.10mg·L-1之间。日间加标回收率在83.7%~114%之间,日间相对标准偏差(n=6)在3.4%~9.8%之间;日内加标回收率在81.9%~113%之间,日内相对标准偏差(n=6)在1.5%~6.7%之间。     

同位素稀释内标-气相色谱-质谱法测定植物油中16种邻苯二甲酸酯的含量

植物油样品0.400 0g,加混合内标溶液20μL混匀,经乙腈4mL超声提取15min。离心后,提取液经活化的SILICA/PSA混合玻璃固相萃取柱净化。净化液经氮气吹干后,残渣用正己烷溶解并稀释至1.0mL。待测液采用DB-5MS UI色谱柱进行气相色谱分离,采用电子轰击离子源和选择离子监测模式进行质谱分析,同位素内标法定量。16种邻苯二甲酸酯类化合物的线性范围均在0.01~1.00mg·L~(-1)之间,检出限(3S/N)在0.003 0~0.035mg·kg~(-1)之间,按标准加入法在3个浓度水平上进行回收试验,回收率在81.7%~113%之间,测定值的相对标准偏差(n=6)在2.8%~11%之间。     

气相色谱-质谱法测定洗涤用品中6种邻苯二甲酸酯

建立了测定洗涤用品中6种邻苯二甲酸酯的气相色谱-质谱法。样品经乙酸乙酯超声提取5min,提取液在HP-5MS毛细管色谱柱上分离,质谱分析中采用电子轰击离子源和选择离子监测模式,外标法定量。6种邻苯二甲酸酯的线性范围为1.0~20mg·L~(-1),方法的检出限(3S/N)均小于1.0mg·kg~(-1);样品中6种邻苯二甲酸酯的加标回收率在85.6%~113%之间,测定值的相对标准偏差(n=6)在2.2%~5.8%之间。     

固相萃取-气相色谱-质谱法同时测定植物油中7种邻苯二甲酸酯

采用气相色谱-质谱法测定植物油中7种邻苯二甲酸酯类增塑剂的含量。样品用正己烷溶解后,经Cleanert PAE固相萃取柱净化,采用正己烷-乙酸乙酯(1+1)混合溶液洗脱,洗脱液用氮气吹至近干,乙腈定容后,在DB-5毛细管色谱柱上分离,质谱中选择电子轰击离子源-选择离子监测模式。7种邻苯二甲酸酯的质量浓度在0.1~5.0 mg·L-1范围内呈线性,检出限(3S/N)为0.02 mg·kg-1。加标回收率在80.0%~120%之间,测定值的相对标准偏差(n=6)在1.1%~5.4%之间。     

气相色谱-串联质谱法测定生态纺织品中的邻苯二甲酸酯类

采用气相色谱-串联质谱法同时测定生态纺织品中的24种邻苯二甲酸酯类。样品经正己烷超声提取,提取液经ProElut PSX玻璃固相萃取柱净化,以丙酮-正己烷(15+85)混合液洗脱,洗脱液经氮气吹至近干后,用正己烷定容至1.0 mL。采用DB-5MS毛细管色谱柱分离,质谱分析中采用电子轰击离子源和选择反应监测模式。24种邻苯二甲酸酯类的质量浓度在一定范围内与峰面积呈线性关系,检出限(3S/N)在1.0~10 mg·kg~(-1)之间,测定下限(10S/N)在5.0~25 mg·kg~(-1)之间。加标回收率在81.3%~102%之间,测定值的相对标准偏差(n=6)在1.8%~6.6%之间。     

气相色谱-质谱法测定汽油中8种醚类和苯胺类添加剂

采用气相色谱-质谱法同时测定汽油8种醚类和苯胺类化合物。采用强极性离子液体色谱柱(SLB-1L 111毛细管色谱柱)分离样品,质谱中选择电喷雾离子源-选择离子监测模式,以苯乙酮为内标物进行定量分析。8种化合物的质量分数在10~10 000 mg·kg-1范围内与其峰面积呈线性关系,检出限(3S/N)在0.2~2.0 mg·kg-1之间。加标回收率在91.2%~111%之间,测定值的相对标准偏差(n=7)在0.18%~3.0%之间。     

超声萃取分离-气相色谱-质谱法测定土壤中的3种酰胺类化合物含量

采用超声萃取-气相色谱-质谱法测定土壤中N,N-二甲基甲酰胺、N,N-二甲基乙酰胺和N,N-二甲基丙烯酰胺等3种酰胺类化合物的含量。样品经丙酮超声提取,在气相色谱分离中用DB-624色谱柱为固定相,在质谱分析中采用全扫描和选择离子监测模式。3种酰胺类化合物的质量浓度均在0.05~20.0mg·L~(-1)范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.5~1.5mg·kg~(-1)之间。加标回收率在85.3%~110%之间,测定值的相对标准偏差(n=7)在1.5%~5.3%之间。     

α-Amino acid derived enaminones and their application in the synthesis of N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates and other heterocycles

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.     

Specific intramolecular aromatic CH insertion of diazosulfonamides

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.     

N-Heterocyclic carbene-palladacyclic complexes: synthesis,characterization and their applications in the C-N coupling and α-arylation of ketones using aryl chlorides

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%).     

Iodine-mediated oxidative Pictet-Spengler reaction using terminal alkyne as the 2-oxoaldehyde surrogate for the synthesis of 1-aroyl-β-carbolines and fused-nitrogen heterocycles

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.     

Facile synthesis of bicyclic 1-arylpyrazol-5-ones

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.     

Synthesis of pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles by Curtius reaction in Morita-Baylis-Hillman derivatives

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.     

正丁胺对激光染料荧光谱影响的研究

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.     

Cu0-catalysed 1,3-dipolar cycloadditions of α-amino acid derived N,N-cyclic azomethine imines to ynones

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 Cu^I 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).     

Synthesis and antioxidative/anti-inflammatory activity of novel fullerene–polyamine conjugates

(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.