摘要
利用毛细管电泳（capillary electrophoresis,CE）仪结合紫外-可见光二极管阵列检测器检测技术建立水体中痕量微囊藻毒素的检测新方法。通过与GB/T 20466—2006《水中微囊藻毒素的测定》高效液相色谱（high performance liquid chromatography,HPLC）方法对比分析,进行2种检测技术的评价。CE检测条件为：毛细管柱（60 cm×75μm i.d.）,有效长度为44 cm,分离缓冲溶液为12 mmol/L硼酸盐（p H 9.0）,分离电压25 kV,检测波长238 nm,压力6 895 Pa流体动力学进样;优化后的HPLC检测条件为：C18色谱柱（250 mm×4.6 mm i.d.,5μm）,甲醇-磷酸盐缓冲溶液（60∶40,V/V）为流动相,检测波长238 nm,柱温度35℃,流速1 m L/min。结果表明：CE对3种微囊藻毒素MC-RR、MC-LR和MC-YR的检出限分别是0.16、0.20μg/m L和0.24μg/m L,HPLC对3种微囊藻毒素的检出限分别为0.020、0.079μg/m L和0.052μg/m L,这2个方法的灵敏度相差1个数量级;加标回收率分别92.5%-106.0%和99.6%-102.5%,CE对应的保留时间和峰面积的精密度相对标准偏差为0.53%-0.64%和2.67%-3.29%;HPLC法的保留时间和峰面积精密度相对标准偏差为0.16%-0.53%和0.80%-1.53%。检测同一水样中微囊藻毒素含量,CE检测结果和HPLC结果之间差异不显著（P〉0.05）。
A new method for the detection of trace amounts of microcystins（MCs） in drinking water sources by capillary electrophoresis（CE） coupled with ultraviolet/visible light diode array detector（DAD） system was established and compared with the high performance liquid chromatography（HPLC） described in the Chinese standard method（GB/T 20466—2006）. CE detection conditions were determined as follows： an uncoated fused-silica capillary tube（60 cm × 75 μm i.d.） with effective length of 44 cm as stationary phase, 12 mmol/L sodium borate solution（p H 9.0） as running buffer, separation voltage of 25 k V, sample injection under 6 895 Pa for 5 s, and detection wavelength of 238 nm. The HPLC method was performed with a C18 chromatographic column（250 mm × 4.6 mm i.d., 5 μm） using methanol： phosphate buffer solution（60：40, V/V） as mobile phase at a flow rate of 1 m L/min. The column temperature was set at 35 ℃, and the analyte was detected at 238 nm. The limits of detection（LOD） of the CE method for MC-RR, MC-LR and MC-YR were 0.16, 0.20 and 0.24 μg/m L, and those of the HPLC method were 0.020, 0.079, and 0.052 μg/m L, respectively. The sensitivity of the two methods differed by 1 order of magnitude. The recoveries of the CE and HPLC methods for three MCs were in range of 92.5%–106.0% and 99.6%–102.5%, respectively. The corresponding relative standard deviations（RSDs） of retention time and peak area were 0.53%–0.64% and 2.67%–3.29% for CE and 0.16%–0.53% and 0.80%–1.53% for HPLC, respectively. For the same water sample, the MCs content determined by CE was not significantly different from that determined by HPLC（P〈0.05）.
作者
王阳
徐明芳
曾晓琮
耿梦梦
黎明
陈耕南
WANG Yang XU Mingfang ZENG Xiaocong GENG Mengmeng LI Ming CHEN Gengnan(College of Life Science and Technology, Jinan University, Guangzhou 510632, China Research Center of Emergency Management, Jinan University, Guangzhou 510632, China Guangdong Provincial Institute of Food Inspection, Guangdong Provincial Wine Testing Center, Guangzhou 510435, China)
出处
《食品科学》
EI
CAS
CSCD
北大核心
2016年第22期210-215,共6页
Food Science
基金
暨南大学应急管理研究中心重大项目(JD2015008)
广东省科技计划项目(2009B011300003)
关键词
高效毛细管电泳
高效液相色谱
微囊藻毒素
检测
capillary electrophoresis（CE）
high performance liquid chromatography（HPLC）
microcystins（MCs）
detection
