高效液相色谱-串联质谱法检测河豚毒素的方法研究

目的建立了一种河豚中河豚毒素(TTX)的高效液相色谱-串联质谱检测方法。方法取适量样品,在0.03 mol/L乙酸溶液中均质后超声提取样品中的河豚毒素。粗提液低速离心,取上清液加入等量甲醇充分混匀后进行高速离心。高速离心后上清液过0.22μm滤膜后待测。采用Waters ACQUITY UPLC BEH Amide(2.1mm×100 mm,1.7μm)色谱分析柱,含0.1%甲酸的Milli Q水及乙腈溶液为流动相,电喷雾正离子模式进行分析。结果河豚毒素在5~1000 ng/m L的范围内线性关系良好,相对回收率为83.3%~93.2%,绝对回收率为47.8%~48.9%,检出限为5μg/kg,定量限为2 0μg/kg。结论 与以往检测TTX的LC-MS/MS方法相比,新建方法操作简单、快速、准确、灵敏并且实验成本低,为河豚中TTX的定量检测提供了有效的实用技术手段。

离子色谱技术在污水监测中的应用和发展趋势

从前处理技术、色谱柱、淋洗系统、抑制器和检测项目等方面,分析总结了自20世纪80年代以来离子色谱技术在污水监测中的应用情况,并结合离子色谱技术的最新发展,分析了离子色谱技术在污水监测中的发展趋势。

高效液相色谱法测定全麦粉中呕吐毒素含量

对高效液相色谱法测定全麦粉中呕吐毒素含量进行了研究,分析了前处理方法、提取方式和提取时间、标准曲线及色谱柱等因素对全麦粉中呕吐毒素含量测定结果的影响。结果表明:与多功能净化柱法相比,对于样品提取液色泽深的陈麦粉,采用0.1%吐温洗脱添加样品后的免疫亲和柱,样品处理干净,色谱图杂峰少,利于目标峰分离;与GB5009.111—2016中的色谱测定条件相比,C18,5mm 4.6×250 mm型号的色谱柱更适用于全麦粉中呕吐毒素含量的测定。

Analysis of the monosaccharide composition of fucoidan by precolumn derivation HPLC

We developed an HPLC method for analysis of the monosaccharide composition of fucoidans. The fucoidan was hydrolyzed into monosaccharides with 2 mol/L trifluoroacetic acid. Using ribose as the internal standard, the monosaecharide derivatives, obtained with 1-Phenyl-3-methyl-5- pyrazolone （PMP）, were separated by reverse-phase HPLC using a gradient elution process, and monitored by ultraviolet detection at 245 nm. In the concentration range of 0.1-2.0 mmol/L, the peak area of each monosaccharide had a good linear relationship with its concentration （r^2〉0.998）. The average recoveries of mannose, rhamnose, glucuronic acid, glucose, galactose, xylose, and fucose were 86.2%, 95.1%, 62.5%, 102.0%, 94.8%, 66.6%, and 105.1%, respectively. This method was accurate and had good reproducibility and could be used to determine the monosaccharide contents of fucoidans.