反相离子对液相色谱-二极管阵列检测器测定红薯粉条中溴酸钾

摘要

[目的]建立反相离子对液相色谱-二极管阵列检测器测定红薯粉条中溴酸钾的分析方法.[方法]样品以超纯水超声波提取,加入甲醇混合后离心,取上清液微孔滤膜过滤作为供试品液.使用Waters Symmetry shieldTM RP18色谱柱,以甲醇∶水(含4.0 mmol/L 柠檬酸与0.5 mmol/L十六烷基三甲基溴化铵溶液,pH为4.5)40∶60(V/V)为流动相,二极管阵列检测器扫描检测,以保留时间和190~400 nm光谱定性,210 nm波长下溴酸钾峰面积定量.[结果]溴酸钾在5.135~ 513.500 μg/mL浓度范围内线性关系良好,相关系数大于0.999,方法回收率在83.5%~88.5%,检出限为0.9 mg/kg,定量限为2.5 mg/kg.[结论]该方法简单、快速、可靠、灵敏、高效,可用于红薯粉条中溴酸钾的分析检测.%[Objective] To establish a method for determination of potassium bromate in sweet potato vermicelli by ion-pair RP-HPLC with diode array detector.[Method] The samples were extracted with ultra pure water by ultrasonic,mixed with methanol and centrifuged,supernatant solution was filtrated by microporous membrane as tested solution.The separation and determination were based on a Waters Symmetry shieldTM RP18 column with UV detector at 210 nm and methanol∶liquid (40∶60) of 4.0 mmol/L citric acid at 0.5 mmol/L hexadecyl-trimethylammonium bromide(pH 4.5) as mobile phase.[Result] The calibration curve was linear in the range of 5.135 to 513.500 μg/mL and the correlation coefficients were greater than 0.999,while the recovery was from 83.5% to 88.5%.The limit of detection (LOD) and the limit of quantitation (LOQ) were 0.9 mg/kg and 2.5 mg/kg separately in this method.[Conclusion] The method is simple,rapid,reliable,sensitive and efficient,and can be used for the detection of potassium bromate in sweet potato vermicelli.