首页|基质分散固相萃取结合超高效液相色谱-串联质谱法快速测定红糖中丙烯酰胺

基质分散固相萃取结合超高效液相色谱-串联质谱法快速测定红糖中丙烯酰胺

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该研究建立了一种基质分散固相萃取结合超高效液相色谱-串联质谱法快速测定红糖中丙烯酰胺的方法.样品加入13C3-丙烯酰胺同位素内标并用水-乙腈溶解,经盐析作用提取到乙腈中,分离乙腈层后,采用SCX+PSA净化,最后利用超高效液相色谱-串联质谱法测定,内标法定量.结果表明,丙烯酰胺在1.0~200 ng·mL-1范围内线性关系良好(r2=0.9994),方法检出限(LOD)和定量限(LOQ)分别为0.78 μg·kg-1和2.62μg·kg-1.对两份红糖样品进行6个浓度水平的加标验证,平均回收率介于95.0~99.2%之间,相对标准偏差(RSD)在1.0~2.2%之间.采集不同产地、品牌和性状的红糖样品19份,结果介于136.3~2011.5μg·kg-1之间,多集中在400 μg·kg-1附近,存在一定的安全风险.
Rapid determination of acrylamide in brown sugar by matrix dispersion solid phase extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry
In this study,a method for rapid determination of acrylamide in brown sugar by matrix dispersion solid phase extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.The sam-ple was added to the internal standard of 13 C3-acrylamide isotope and dissolved in water-acetonitrile.It was extracted into acetoni-trile by salting.After the acetonitrile layer was separated,it was purified by SCX+PSA,and finally determined by UPLC-MS/MS,and the internal standard method was used for measurement.The results show that acrylamide has a good linear relationship in the range of 1.0~200 ng·mL-1(r2=0.9994),and the detection limit(LOD)and quantitative limit(LOQ)of the method are 0.78 μg·kg-1 and 2.62 μg·kg-1.19 brown sugar samples of different origins,brands and traits were collected,and the results were be-tween 136.3 and 2011.5 μg·kg-1,mostly concentrated near 400 μg·kg-1,which has certain safety risks.

matrix dispersion solid phase extractionbrown sugaracrylamideultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)

徐曼、张耀恬、王银、胡俊、吴德

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克拉玛依市疾病预防控制中心,新疆 克拉玛依 834000

成都中医药大学公共卫生学院,四川 成都 611137

基质分散固相萃取 红糖 丙烯酰胺 超高效液相色谱-串联质谱法

2025

化学研究与应用
四川省化学化工学会 四川大学

化学研究与应用

北大核心
影响因子:0.555
ISSN:1004-1656
年,卷(期):2025.37(1)