作者：黄泽玮, 刘忠莹, 黄瑛, 杜钢, 贺亚玲
作者单位：四川省食品药品检验检测院, 四川 成都 611731
关键词：Orbitrap-Elite高分辨质谱;非法添加;快速筛查;减肥;壮阳
摘要：
建立基于Orbitrap-Elite高分辨质谱的快速筛查及确证减肥及壮阳类保健食品和中成药中54种非法添加物的方法。采用Hypersil GOLD C18 column色谱柱（150 mm×2.1 mm，1.9 μm），梯度洗脱，流量0.3 mL/min，正离子全扫描/数据依赖的二级扫描模式，在28 min内完成54种目标化合物的分离和高精度一级、二级质谱扫描，并通过Exact Finder 2.0软件进行快速筛查，以确证样品中是否掺加减肥及壮阳类化学药物。结果显示在28 min内54种化合物能得到较好分离；6种基质加标溶液中54种化合物的一级与二级离子精确质量数的实测值与理论值均在5×10-6误差之内；空白溶液中54种化合物结果均为阴性；20批减肥及壮阳类保健食品及中成药样品中检出1批阳性样品，阳性率5%。该方法操作简单快捷，结果定性准确，无假阴性和假阳性情况出现，可用于减肥及壮阳类保健食品和中成药中54种非法添加的高通量快速筛查及确证。
Application of Orbitrap-Elite high resolution mass spectrometry for the rapid screening and confirmation of 54 illegal additives in healthy food and herbal medicines for slimming and anti-impotence
HUANG Zewei, LIU Zhongying, HUANG Ying, DU Gang, HE Yaling
Sichuan Institute for Food and Drug Control, Chengdu 611731, China
Abstract: To establish an Orbitrap-Elite high resolution mass spectrometry method for the screening and confirmation of 54 illegal additives in healthy food and herbal medicines for slimming and anti-impotence.The analytes were separated on a Hypersil GOLD C18 chromatographic column (150 mm×2.1 mm, 1.9 μm) and by gradient elution at a flow rate of 0.3 mL/min. The positive-ion electron spray ionization(ESI), Full MS/data-dependent MS2 mode and Exact Finder 2.0 software were used to screen the accurate MS and MS2 fragment ions during 28 minutes. 54 analytes can be well separated during 28 minutes. In the six matrix solutions with standard addition, the measured values and theoretical values of the MS and MS2 fragment ions of the 54 compounds were within the error of 5×10-6. In the blank solution, the results of 54 compounds were all negative. Among 20 kinds of healthy food and herbal medicine, 5% of the studied samples were positive. This new Orbitrap-Elite HRMS method is simple and fast, and the result is qualitatively accurate with no false negative or false positive, which provides a novel powerful tool for the high-throughput rapid screening and confirmation of 54 illegal additives in healthy food and herbal medicines for slimming and anti-impotence.
Keywords: Orbitrap-Elite high resolution mass spectrometry (HRMS);illegal additives;rapid screening;slimming;anti-impotence
2019, 45(1):70-76 收稿日期: 2018-07-12;收到修改稿日期: 2018-08-23
基金项目: 四川省科技厅重点研发项目（2018SZ0340）
作者简介: 黄泽玮(1986-),男,四川内江市人,主管药师,硕士,主要从事食品理化检测
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