食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
FOOD SAFETY AND QUALITY DETECTION TECHNOLOGY
2013年
1期
239-244
,共6页
曾绍东%杜海群%郭宏斌%王明月*%查玉兵
曾紹東%杜海群%郭宏斌%王明月*%查玉兵
증소동%두해군%곽굉빈%왕명월*%사옥병
超高压液相色谱-串联质谱%甜蜜素%糖精钠%安赛蜜%水果
超高壓液相色譜-串聯質譜%甜蜜素%糖精鈉%安賽蜜%水果
초고압액상색보-천련질보%첨밀소%당정납%안새밀%수과
ultra-high pressure liquid chromatography-mass spectrometry%sodium cyclamate%saccharin sodium%acesulfame%fruits
目的建立水果中3种人工合成甜味剂(甜蜜素、糖精钠、安赛蜜)的超高压液相色谱-串联质谱(UPLC-MS/MS)检测方法.方法以反相C18柱为色谱柱,乙腈?0.02 mol/L乙酸铵溶液为流动相,样品经纯水提取后用色谱柱进行分离,串联质谱负离子多反应监测(MRM)模式测定.结果3种人工合成甜味剂在10~600μg/L范围内响应峰面积和样品质量浓度之间有良好的线性关系(相关系数r≥0.995);甜蜜素、糖精钠和安赛蜜的最低检出限分别为0.8、5.0、1.0μg/kg;在2种添加水平下,样品平均回收率为74.9%~111.2%,相对标准偏差<8%.结论该方法前处理简单,分析时间短,具有良好的灵敏度和准确性,可用于水果中甜蜜素、糖精钠、安赛蜜的同时检测.
目的建立水果中3種人工閤成甜味劑(甜蜜素、糖精鈉、安賽蜜)的超高壓液相色譜-串聯質譜(UPLC-MS/MS)檢測方法.方法以反相C18柱為色譜柱,乙腈?0.02 mol/L乙痠銨溶液為流動相,樣品經純水提取後用色譜柱進行分離,串聯質譜負離子多反應鑑測(MRM)模式測定.結果3種人工閤成甜味劑在10~600μg/L範圍內響應峰麵積和樣品質量濃度之間有良好的線性關繫(相關繫數r≥0.995);甜蜜素、糖精鈉和安賽蜜的最低檢齣限分彆為0.8、5.0、1.0μg/kg;在2種添加水平下,樣品平均迴收率為74.9%~111.2%,相對標準偏差<8%.結論該方法前處理簡單,分析時間短,具有良好的靈敏度和準確性,可用于水果中甜蜜素、糖精鈉、安賽蜜的同時檢測.
목적건립수과중3충인공합성첨미제(첨밀소、당정납、안새밀)적초고압액상색보-천련질보(UPLC-MS/MS)검측방법.방법이반상C18주위색보주,을정?0.02 mol/L을산안용액위류동상,양품경순수제취후용색보주진행분리,천련질보부리자다반응감측(MRM)모식측정.결과3충인공합성첨미제재10~600μg/L범위내향응봉면적화양품질량농도지간유량호적선성관계(상관계수r≥0.995);첨밀소、당정납화안새밀적최저검출한분별위0.8、5.0、1.0μg/kg;재2충첨가수평하,양품평균회수솔위74.9%~111.2%,상대표준편차<8%.결론해방법전처리간단,분석시간단,구유량호적령민도화준학성,가용우수과중첨밀소、당정납、안새밀적동시검측.
Objective To establish a method for the determination of three synthetic sweeteners(sodium cyclamate, saccharin sodium, and acesulfame) in fruits by ultra-high pressure liquid chromatography-mass spectrometry (UPLC-MS/MS). Methods The synthetic sweeteners were extracted with water, separated on a reversed phase C18 column using acetonitrile-0.02mol/L ammonium acetate as mobile phase, and then detected by UPLC-MS/MS under multiple reaction monitoring (MRM) mode. Results The method showed a good linearity for all the analysts over the range of 10~600μg/L with r≥0.995. The detection limits of sodium cy-clamate, saccharin sodium and acesulfame were 0.8、5.0 μg/kg and 1.0 μg/kg, respectively. The recoveries ranged from 74.9% to 111.2% at two spiked concentrations with the relative standard deviations lower than 8%.Conclusion This established method has the advantages of easy to operate, fast to perform, with high sensitivity and accuracy, and it is suitable for detection of sodium cyclamate, saccharin sodium and acesulfame in fruits.