UHPLC-MS/MS Determination of Advantame in Compound Seasoning with Purification by QuEChERS
摘 要
称取复合调味料样品1.000 0 g,用甲醇-水(50+50)溶液作为提取剂将样品中爱德万甜溶于提取剂中。先后提取2次,每次加提取剂10 mL,振荡提取10 min,高速离心5 min。收集2次上清液,合并并用水定容至25.0 mL。分取此溶液1.0 mL加入于已装有C18 200 mg和N-丙基乙二胺(PSA)100 mg的EP管中,涡旋混匀1 min,高速离心2 min,取上清液经0.22 μm滤膜过滤。分取滤液5 μL进样,以Agilent ZORBAX SB-C18色谱柱作为固定相,以不同比例的0.1%(体积分数)甲酸溶液(A)和甲醇(B)的混合液作为流动相,按程序进行梯度洗脱。串联质谱分析中采用电喷雾离子源正离子扫描和多反应监测模式。测得爱德万甜的线性范围在0.2~20 μg·L-1之间,其检出限(3S/N)为2.0 μg·kg-1。以调味粉和调味酱样品作为基体,用标准加入法进行回收和精密度试验,测得回收率在89.3%~98.5%之间,测定值的相对标准偏差(n=6)在1.8%~3.8%之间。
Abstract
A portion (1.000 0 g) of compound seasoning sample was extracted twice with mixed solvent of CH3OH and H2O (50+50) to transfer the analyte, advantame, from the sample into solution. 10 mL of the mixed solvent was used in each extraction, which was performed by swirling for 10 min and centrifuging for 5 min with high speed. Supernatants from the 2 extractions were collected and diluted to 25.0 mL with water. An aliquot of 1.0 mL of the solution was mixed by swirling for 1 min with 200 mg of C18 and 100 mg of PSA in an EP tube and centrifuged for 2 min with high speed for purification. The supernatant was filtered through 0.22 μm filtering membrane and 5 μL of the filtrate was introduced into the instrument by using Agilent ZORBAX SB-C18 column as stationary phase and using mixtures of 0.1% (φ) formic acid solution (A) and CH3OH (B) mixed in various rations as mobile phases in the programed gradient elution. ESI with positive ion scanning mode and mode of MRM were adopted in MS/MS. Linearity range for advantame was found between 0.2 to 20 μg·L-1, with detection limit (3S/N) of 2.0 μg·kg-1. Using powdery and pasty seasoning samples as matrixes, tests for recovery and precision were made by standard addition method, giving values of recovery in the range of 89.3% to 98.5%, and values of RSDs (n=6) in the range of 1.8% to 3.8%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201909007
所属栏目 工作简报
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收稿日期 2019/1/10
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备注张小刚,硕士,研究方向为食品质量与安全
引用该论文: ZHANG Xiaogang,WANG Xia,WANG Weidong,FAN Yanhong,SUN Hongfeng. UHPLC-MS/MS Determination of Advantame in Compound Seasoning with Purification by QuEChERS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(9): 1023~1027
张小刚,王霞,王卫东,范艳红,孙洪峰. QuEChERS净化-超高效液相色谱-串联质谱法测定复合调味料中的爱德万甜含量[J]. 理化检验-化学分册, 2019, 55(9): 1023~1027
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参考文献
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【13】贾玮,黄峻榕,凌云,等.高效液相色谱-串联质谱法同时测定茶叶中290种农药残留组分[J].分析测试学报, 2013,32(1):9-22.
【14】LIU M, XIE Y, LI H C, et al. Multiresidue determination of 29 pesticide residues in pepper through a modified QuEChERS method and gas chromatography-mass spectrometry[J]. Biomedical Chromatography, 2016,30(10):1686-1695.
【15】曲斌,朱志谦,陆桂萍,等.UPLC-MS/MS快速测定鸡肉中金刚烷胺和氟喹诺酮类药物残留[J].中国兽药杂志, 2013,47(7):50-54.
【16】郭伟,刘永,刘宁,等.超高效液相色谱串联质谱分析牛乳中24种磺胺类药物残留[J].分析化学, 2009,37(11):1638-1644.
【17】SCHWAIGER B, KÖNIG J, LESUEUR C. Development and validation of a multi-class UHPLC-MS/MS method for determination of antibiotic residues in dairy products[J]. Food Analytical Methods, 2018,11(5):1417-1434.
【2】FDA. Food additives permitted for direct addition to food for human consumption; advantame.[EB/OL]. (2014-12-14)[2019-01-10]. https://www.federalregister.gov/documents/2014/12/24/2014-30144/food-additives-permitted-for-direct-addition-to-food-for-human-consumption-advantame.
【3】EFSA. Scientific opinion on the safety of advantame for the proposed uses as a food additive[J]. EFSA Journal, 2013,11(7):3301-3369.
【4】国家卫生计生委.关于爱德万甜等6种食品添加剂新品种、食品添加剂环己基氨基磺酸钠(又名甜蜜素)等6种食品添加剂扩大用量和使用范围的公告[EB/OL].(2017-10-20)[2018-10-19]. http://www.moh.gov.cn/sps/s7890/201710/c4cc46c01005445f88ad169c8e820aee.shtml.
【5】陈健,林真,钱疆,等.高效液相色谱法检测饮料中艾德万甜含量[J].食品安全质量检测学报, 2016,7(12):4853-4857.
【6】汪辉,曹阳,曹雄杰,等.高效液相色谱法测定食品中的爱德万甜[J].分析测试学报, 2018,37(5):635-638.
【7】廖燕芝,秦海蛟,徐文泱,等.超高效液相色谱-串联质谱法检测食品中爱德万甜[J].中国食品添加剂, 2018(9):198-201.
【8】汪辉,黄小贝,刘江,等.超高效液相色谱-串联质谱快速测定食品中的新品种甜味剂爱德万甜[J].色谱, 2018,36(7):700-704.
【9】公丕学,杨昊,廉贞霞,等.固相萃取-超高效液相色谱质谱法测定液体乳中爱德万甜[J].中国调味品, 2018,43(6):159-164.
【10】KOBAYASHI M, TERADA H, NAKAJIMA M. Determination method of ultra-high-intensity sweetener, advantame, in processed foods by HPLC and LC-MS/MS[J]. Shokuhin Eiseigaku Zasshi, 2015,56(1):14-18.
【11】KOKOTOU M G, THOMAIDIS N S. Characterization of the retention of artificial sweeteners by hydrophilic interaction liquid chromatography[J]. Analytical Letters, 2018,51(1/2):49-72.
【12】张爱芝,王全林,曹丽丽,等.QuEChERS-超高效液相色谱-串联质谱法测定蔬菜中250种农药残留[J].色谱, 2016,34(2):158-164.
【13】贾玮,黄峻榕,凌云,等.高效液相色谱-串联质谱法同时测定茶叶中290种农药残留组分[J].分析测试学报, 2013,32(1):9-22.
【14】LIU M, XIE Y, LI H C, et al. Multiresidue determination of 29 pesticide residues in pepper through a modified QuEChERS method and gas chromatography-mass spectrometry[J]. Biomedical Chromatography, 2016,30(10):1686-1695.
【15】曲斌,朱志谦,陆桂萍,等.UPLC-MS/MS快速测定鸡肉中金刚烷胺和氟喹诺酮类药物残留[J].中国兽药杂志, 2013,47(7):50-54.
【16】郭伟,刘永,刘宁,等.超高效液相色谱串联质谱分析牛乳中24种磺胺类药物残留[J].分析化学, 2009,37(11):1638-1644.
【17】SCHWAIGER B, KÖNIG J, LESUEUR C. Development and validation of a multi-class UHPLC-MS/MS method for determination of antibiotic residues in dairy products[J]. Food Analytical Methods, 2018,11(5):1417-1434.
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