建立了一种同时检测湿巾中5种噻唑啉酮类防腐剂的高效液相色谱方法。该方法以甲醇作为萃取溶剂,涡旋振荡,室温下超声萃取湿巾中的防腐剂。萃取液浓缩后,定容,采用高效液相色谱法分析,外标法定量。5种噻唑啉酮类防腐剂的色谱分离在Eclips...建立了一种同时检测湿巾中5种噻唑啉酮类防腐剂的高效液相色谱方法。该方法以甲醇作为萃取溶剂,涡旋振荡,室温下超声萃取湿巾中的防腐剂。萃取液浓缩后,定容,采用高效液相色谱法分析,外标法定量。5种噻唑啉酮类防腐剂的色谱分离在Eclipse Plus C18色谱柱完成,采用梯度洗脱方式,流动相为0.05 mol/L磷酸二氢钠缓冲液/甲醇。通过5种目标化合物各自的保留时间进行定性,色谱图的峰面积进行定量。在一定的线性范围内,每种目标化合物的峰面积均与其质量浓度呈线性相关关系,相关系数均不小于0.9990。在3个不同的添加浓度水平下,加标回收率在82.0%~102.0%之间,相对标准偏差值(n=6)均不大于3.07%。该方法操作简便,应用范围广,分析时间短,灵敏度高,基质适用性好,可完全满足湿巾中噻唑啉酮类防腐剂检测工作的需要。展开更多
A novel pyridine-contained a-cyanostilbenzene Schiff base, （Z）-3-（4-butoxy- phenyl）-2-（4-（（E）-pyridin-2-yl-methyleneamino）phenyl）acrylonitrile （L）, has been synthesized and characterized by 1H NMR, 13C NMR...A novel pyridine-contained a-cyanostilbenzene Schiff base, （Z）-3-（4-butoxy- phenyl）-2-（4-（（E）-pyridin-2-yl-methyleneamino）phenyl）acrylonitrile （L）, has been synthesized and characterized by 1H NMR, 13C NMR, FT-IR spectra and single-crystal X-ray diffraction. Single-crystal data show that compound L belongs to the triclinic system, space group P1, with a = 8.759（4）, b = 10.779（4）, c = 12.594（5） A, a= 65.873（4）, β = 88.332（5）, 7= 73.800（5）°, M,. = 381.46, V= 1037.2（7） A3, Z = 2, Dc = 1.221 g/cm-3,μ = 0.076 mm-1, F（000） = 404, gint = 0.0311, R （I〉 20（I）） = 0.0484, wR （I 〉 20（I）） = 0.1544, R （all data） = 0.0484, wR （all data） = 0.1692, completeness to theta = 25.000 being 99.0% and GOF = 1.179. There are two kinds of intermolecular hydrogen bonds and one kind of C-H……π weak interaction between adjacent molecules. Compound L can be used as a candidate for desirable devices with high performance due to its good thermal stability and excellent optical performance.展开更多
Researches on a-cyanostilbene derivatives demonstrated them to be promising AIE or AIEE structural molecules and potential photoelectric materials. One novel a-cyanostilbene derivative, namely （E）-2-（4-butoxyphenyl...Researches on a-cyanostilbene derivatives demonstrated them to be promising AIE or AIEE structural molecules and potential photoelectric materials. One novel a-cyanostilbene derivative, namely （E）-2-（4-butoxyphenyl）-3-（4-（diethylamino）phenyl）acrylonitrile （BPDPA）, has been designed, synthesized and characterized. The crystalline structure of BPDPA has been studied in detail. The single-crystal X-ray diffraction revealed BPDPA crystallizes in triclinic space group Pi, with a = 12.860（5）, b = 13.327（5）, c = 15.016（5）А, a = 72.650（5）, β = 66.969（5）, Y = 62.897（5）°, Mr = 696.95, V= 2085.6（13） A3, Z = 2, Dc = 1.110 g/cm-3, p = 0.068 mm1, F（000） = 752, Rint = 0.0264, R（I〉 2σ（/）） = 0.0649, wR（l〉 2σ（/） = 0.1724, R（all data） = 0.1321, wR （all data） = 0.2158, completeness to theta = 25.00 is 99.4% and GOF = 1.067. Like most reported a-cyanostilbene derivatives, BPDPA possesses a somewhat twisted molecular structure. UV-Vis and FL measurements showed an obviously bathochromic effect of BPDPA with increasing the polarity of the solvents.展开更多
文摘建立了一种同时检测湿巾中5种噻唑啉酮类防腐剂的高效液相色谱方法。该方法以甲醇作为萃取溶剂,涡旋振荡,室温下超声萃取湿巾中的防腐剂。萃取液浓缩后,定容,采用高效液相色谱法分析,外标法定量。5种噻唑啉酮类防腐剂的色谱分离在Eclipse Plus C18色谱柱完成,采用梯度洗脱方式,流动相为0.05 mol/L磷酸二氢钠缓冲液/甲醇。通过5种目标化合物各自的保留时间进行定性,色谱图的峰面积进行定量。在一定的线性范围内,每种目标化合物的峰面积均与其质量浓度呈线性相关关系,相关系数均不小于0.9990。在3个不同的添加浓度水平下,加标回收率在82.0%~102.0%之间,相对标准偏差值(n=6)均不大于3.07%。该方法操作简便,应用范围广,分析时间短,灵敏度高,基质适用性好,可完全满足湿巾中噻唑啉酮类防腐剂检测工作的需要。
基金supported by the National Natural Science Foundation of China(21101001)the Educational Commission of Anhui Province(KJ2014ZD02)
文摘A novel pyridine-contained a-cyanostilbenzene Schiff base, （Z）-3-（4-butoxy- phenyl）-2-（4-（（E）-pyridin-2-yl-methyleneamino）phenyl）acrylonitrile （L）, has been synthesized and characterized by 1H NMR, 13C NMR, FT-IR spectra and single-crystal X-ray diffraction. Single-crystal data show that compound L belongs to the triclinic system, space group P1, with a = 8.759（4）, b = 10.779（4）, c = 12.594（5） A, a= 65.873（4）, β = 88.332（5）, 7= 73.800（5）°, M,. = 381.46, V= 1037.2（7） A3, Z = 2, Dc = 1.221 g/cm-3,μ = 0.076 mm-1, F（000） = 404, gint = 0.0311, R （I〉 20（I）） = 0.0484, wR （I 〉 20（I）） = 0.1544, R （all data） = 0.0484, wR （all data） = 0.1692, completeness to theta = 25.000 being 99.0% and GOF = 1.179. There are two kinds of intermolecular hydrogen bonds and one kind of C-H……π weak interaction between adjacent molecules. Compound L can be used as a candidate for desirable devices with high performance due to its good thermal stability and excellent optical performance.
基金Supported by the Natural Science Foundation of Anhui Province(1208085MB21)the National Natural Science Foundation of China(21101001)
文摘Researches on a-cyanostilbene derivatives demonstrated them to be promising AIE or AIEE structural molecules and potential photoelectric materials. One novel a-cyanostilbene derivative, namely （E）-2-（4-butoxyphenyl）-3-（4-（diethylamino）phenyl）acrylonitrile （BPDPA）, has been designed, synthesized and characterized. The crystalline structure of BPDPA has been studied in detail. The single-crystal X-ray diffraction revealed BPDPA crystallizes in triclinic space group Pi, with a = 12.860（5）, b = 13.327（5）, c = 15.016（5）А, a = 72.650（5）, β = 66.969（5）, Y = 62.897（5）°, Mr = 696.95, V= 2085.6（13） A3, Z = 2, Dc = 1.110 g/cm-3, p = 0.068 mm1, F（000） = 752, Rint = 0.0264, R（I〉 2σ（/）） = 0.0649, wR（l〉 2σ（/） = 0.1724, R（all data） = 0.1321, wR （all data） = 0.2158, completeness to theta = 25.00 is 99.4% and GOF = 1.067. Like most reported a-cyanostilbene derivatives, BPDPA possesses a somewhat twisted molecular structure. UV-Vis and FL measurements showed an obviously bathochromic effect of BPDPA with increasing the polarity of the solvents.
