为了考察水产品中二甲苯麝香和酮麝香的残留量,建立了水产品中痕量二甲苯麝香和酮麝香测定的多重吸附同步净化(MASP)-气相色谱-质谱联用法(GC-MS)。以乙腈高速匀浆提取样品,应用 MASP 方法对样品同时进行提取、盐析和净化,并采用...为了考察水产品中二甲苯麝香和酮麝香的残留量,建立了水产品中痕量二甲苯麝香和酮麝香测定的多重吸附同步净化(MASP)-气相色谱-质谱联用法(GC-MS)。以乙腈高速匀浆提取样品,应用 MASP 方法对样品同时进行提取、盐析和净化,并采用 GC-MS 在选择离子监测( SIM)模式下测定水产品中的痕量二甲苯麝香和酮麝香,以基质匹配标准溶液外标法定量。选用 DB-5 MS 石英毛细管柱(30 m×0.25 mm×0.25μm),采用电子轰击电离源,二甲苯麝香的选择监测离子为 m / z 282、297、265,酮麝香为 m / z 279、294、191。结果表明:在优化条件下,二甲苯麝香和酮麝香在1~100μg / kg 范围内线性良好,相关系数不低于0.999,检出限(S / N =3)为0.30μg / kg。明虾、花蛤和鳗鱼空白样品中1.0、2.0、10.0μg / kg 3个添加水平下二甲苯麝香和酮麝香的加标回收率为79%~104%,相对标准偏差(RSD)为1.6%~13.3%。本方法具有操作简便、快速、准确的特点,可用于水产品中痕量二甲苯麝香和酮麝香的日常检测。展开更多
Total internal reflection fluorescence spectroscopy (TIRF) and synchronous scanning technique were combined to study the adsorption behavior of the meso-tetrakis (4-sulfonatophenyl) porphyrin (TPPS) at the glass-water...Total internal reflection fluorescence spectroscopy (TIRF) and synchronous scanning technique were combined to study the adsorption behavior of the meso-tetrakis (4-sulfonatophenyl) porphyrin (TPPS) at the glass-water interface without any surfactant. The pH dependence of synchronous fluorescence signal at the interface was analyzed. Both unprotonated (TPPS4-) and diprotonated (H2TPPS2-) forms of TPPS were observed at the interface. But the interface favored the adsorption of. The apparent estimated pKa2 value shifted from 5.00 in the bulk solution to 2.7 at the interface. STIRF provides a good technique to study multi-component systems at the interface.展开更多
文摘为了考察水产品中二甲苯麝香和酮麝香的残留量,建立了水产品中痕量二甲苯麝香和酮麝香测定的多重吸附同步净化(MASP)-气相色谱-质谱联用法(GC-MS)。以乙腈高速匀浆提取样品,应用 MASP 方法对样品同时进行提取、盐析和净化,并采用 GC-MS 在选择离子监测( SIM)模式下测定水产品中的痕量二甲苯麝香和酮麝香,以基质匹配标准溶液外标法定量。选用 DB-5 MS 石英毛细管柱(30 m×0.25 mm×0.25μm),采用电子轰击电离源,二甲苯麝香的选择监测离子为 m / z 282、297、265,酮麝香为 m / z 279、294、191。结果表明:在优化条件下,二甲苯麝香和酮麝香在1~100μg / kg 范围内线性良好,相关系数不低于0.999,检出限(S / N =3)为0.30μg / kg。明虾、花蛤和鳗鱼空白样品中1.0、2.0、10.0μg / kg 3个添加水平下二甲苯麝香和酮麝香的加标回收率为79%~104%,相对标准偏差(RSD)为1.6%~13.3%。本方法具有操作简便、快速、准确的特点,可用于水产品中痕量二甲苯麝香和酮麝香的日常检测。
文摘Total internal reflection fluorescence spectroscopy (TIRF) and synchronous scanning technique were combined to study the adsorption behavior of the meso-tetrakis (4-sulfonatophenyl) porphyrin (TPPS) at the glass-water interface without any surfactant. The pH dependence of synchronous fluorescence signal at the interface was analyzed. Both unprotonated (TPPS4-) and diprotonated (H2TPPS2-) forms of TPPS were observed at the interface. But the interface favored the adsorption of. The apparent estimated pKa2 value shifted from 5.00 in the bulk solution to 2.7 at the interface. STIRF provides a good technique to study multi-component systems at the interface.