高效液相色谱-电感耦合等离子体质谱研究Medaka体内水溶性汞结合蛋白

采用高效液相色谱与电感耦合等离子体质谱联用技术,对不同形态汞暴露后的Medaka肝脏和脑组织中水溶性蛋白进行研究,以体积排阻柱为液相分离柱,流动相为0.15 mol/L NH4Ac,流速为0.5 mL/min.利用电感耦合等离子体质谱对Medaka肝脏和脑组织提取液中铜、锌和汞的含量进行了分析,检出限为0.01～0.0...     

高效液相色谱与原子荧光光谱联用分析海产品中的甲基汞

建立了高效液相色谱-紫外消解-氢化物发生-原子荧光光谱联用测定海产品中甲基汞的方法, 比较了不同溶剂对海产品中甲基汞提取效率的影响. 实验采用质量分数25% (m/V) KOH甲醇溶液, 室温振荡10 h消解样品, CH2Cl2萃取, 再以0.01 mol/L Na2S2O3水溶液反萃取, 并采用HPLC-UV-HG-AFS测定鱼和扇贝萃取液中的甲基汞的含量. 在优化分离和前处理条件下, 平行进样5次10 ng/mL的汞混合标准溶液, 甲基汞、无机汞和乙基汞的色谱峰面积的相对标准偏差(RSDs)分别为4.4%、 3.9%和4.3%, 甲基汞、无机汞和乙基汞的检出限分别为0.069、 0.15和0.046 ng/mL;鱼和扇贝的甲基汞的加标回收率为96±5%和95±5%.     

Speciation analysis of organotin compounds in lard poisoning accident in Jiangxi Province, China

Samples including organotin contaminated lard, urine, blood, and main organs of the poisoned bodies were collected in the incident which took place in Longnan and Dingnan counties, Jiangxi Province, China around the new year's day of 1999. The organotin compounds in these samples were identified and determined by gas chromatography-flame photometric detector (GC-FPD), gas chromatography-mass spectroscopy (GC-MS) and inductively coupled plasma-mass spectroscopy (ICP-MS). Experiments confirmed that tri- and dimethyltin are the main components that caused the poisoning accident. Monomethyltin, dioctyltin and inorganic tin were also found in several samples.     

高效液相色谱-氢化物发生-原子荧光光谱在线联用系统分析中成药中砷化合物形态

建立了高效液相色谱-氢化物发生-原子荧光光谱砷形态分析在线联用系统,考察了不同实验条件对4种砷形态化合物（As^Ⅲ,DMA^Ⅴ,MMA^Ⅴ和As^Ⅴ）分离分析的影响,优化了实验条件.在优化的实验条件下,采用pH 5.8的磷酸盐缓冲溶液为流动相,梯度洗脱,10 min之内4种砷形态达到基线分离.进样20μL,测定4种形态的检出限分别为：As^Ⅲ2.76 ng/mL,DMA^Ⅴ7.37 ng/mL,MMA^Ⅴ2.86 ng/mL和As^Ⅴ5.22 ng/mL,相对标准偏差RSD在2.9%～4.2%之间.该联用系统灵敏度高,准确性好,分离分析了部分市售中成药中的不同砷形态化合物.