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高效液相色谱-串联质谱法测定白砂糖中的氯酸盐和高氯酸盐

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目的:建立高效液相色谱-串联质谱法测定白砂糖中氯酸盐和高氯酸盐的方法.方法:样品经乙腈水振荡超声提取,离心后过膜.用Acclaim Trinity P1 色谱柱对化合物进行分离,以乙腈和 10 mmol·L-1甲酸铵溶液梯度洗脱,在电喷雾负离子选择反应监测模式下检测,用同位素内标法定量.结果:氯酸盐在1.0~50.0 ng·mL-1 线性关系良好,相关系数为 0.999 5;高氯酸盐在 0.5~25.0 ng·mL-1 线性关系良好,相关系数为 0.999 9.氯酸盐的检出限为 0.61 mg·kg-1,回收率为 89.0%~110.0%,精密度为 0.54%~1.21%.高氯酸盐的检出限为 0.38 mg·kg-1,回收率为 86.0%~96.6%,精密度为0.36%~1.02%.结论:该方法的前处理简单快捷,灵敏度高,准确性可靠,稳定性好,可为白砂糖安全检测提供技术手段.
Determination of Chlorate and Perchlorate in White Granulated Sugar by High Performance Liquid Chromatography-Tandem Mass Spectrometry
Objective:To establish a high performance liquid chromatography-tandem mass spectrometry method for the determination of chlorate and perchlorate in white granulated sugar.Method:The samples were extracted by ultrasonic oscillation with acetonitrile water,centrifuged and then coated.The compounds were separated by Acclaim Trinity P1 column and eluted with acetonitrile and 10 mmol·L-1 ammonium formate solution.The compounds were detected by electrospray in anion selective reaction monitoring mode and quantified by isotope internal standard method.Result:Chlorate had a good linear relationship between 1.0 ng·mL-1 and 50.0 ng·mL-1 with a correlation coefficient of 0.999 5,and perchlorate had a good linear relationship between 0.5 ng·mL-1 and 25.0 ng·mL-1 with a correlation coefficient of 0.999 9.The detection limit of chlorate was 0.61 mg·kg-1,the recovery was 89.0%~110.0%,and the precision was 0.54%~1.21%.The detection limit of perchlorate was 0.38 mg·kg-1,the recovery was 86.0%~96.6%,and the precision was 0.36%~1.02%.Conclusion:The pretreatment method is simple,rapid,sensitive,reliable and stable,and can provide technical means for the safety detection of white granulated sugar.

liquid chromatography-mass spectrometrywhite granulated sugarchlorateperchlorate

熊碧玉、杨金伟、陆莉莉、农馥俏

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广西壮族自治区产品质量检验研究院,广西南宁 530200

液相色谱-质谱 白砂糖 氯酸盐 高氯酸盐

2024

食品安全导刊
商业科技质量中心 北京肉类食品协会

食品安全导刊

影响因子:0.065
ISSN:1674-0270
年,卷(期):2024.(7)
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