超高效液相色谱-串联质谱法测定保健食品中7种非法添加的化学镇静剂
UPLC-MS/MS Determination of 7 Illegally Added Chemical Sedatives in Health-Care Food
摘 要
采用固相萃取-超高效液相色谱-串联质谱法测定保健食品中7种非法添加的化学镇静剂的含量。保健食品样品以甲醇为溶剂进行提取,经高速离心处理后,取上清液,经Oasis MCX固相萃取柱净化。所得净化液以Zorbax-SB-C18色谱柱为分离柱,以不同体积比的0.1%(体积分数)甲酸溶液和乙腈混合液为流动相进行梯度洗脱,采用电喷雾正离子源多反应监测模式检测。7种化合物的质量浓度均在0.10~30.0 μg·L-1范围内与其峰面积呈线性关系,方法的测定下限(10S/N)在0.1~2.1 μg·kg-1之间。在0.30,3.0,10.0 μg·L-1等3个浓度水平进行加标回收试验,回收率在76.7%~104%之间,测定值的相对标准偏差(n=6)在2.1%~9.8%之间。
固相萃取
保健食品
化学镇静剂
UPLC-MS/MS
Solid phase extraction
Health-care food
Chemical sedatives
Abstract
UPLC-MS/MS was applied to the determination of 7 illegally added sedative drugs in health foods with solid phase extraction. The health-care food sample was extracted with methanol, and after high-speed centrifugation, the supernatant was taken and purified on Oasis MCX SPE solumn. Zorbax-SB-C18 chromatographic column was used as stationary phase, and mixtures of 0.1% (φ) formic acid solution and acetonitrile in various ratios were used as mobile phase in gradient elution. ESI+ and multi-reaction monitoring were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 7 compounds were kept in the same range of 0.10-30.0 μg·L-1, with lower limits of determination (10S/N) in the range of 0.1-2.1 μg·kg-1. Tests for recovery and precision were made by standard addition method at the concentration levels of 0.30, 3.0, 10.0 μg·L-1, giving values of recovery and RSD′s (n=6) in the ranges of 76.7%-104% and 2.1%-9.8% respectively.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201606003
所属栏目 试验与研究
基金项目 国家自然科学基金(21307051);辽宁省自然科学基 金(2013020152)
收稿日期 2015/11/4
修改稿日期
网络出版日期
作者单位点击查看
备注王璐(1982-),女,辽宁沈阳人,助理研究员,主要 从事食品安全检查工作。
引用该论文: WANG Lu. UPLC-MS/MS Determination of 7 Illegally Added Chemical Sedatives in Health-Care Food[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2016, 52(6): 629～634
王璐. 超高效液相色谱-串联质谱法测定保健食品中7种非法添加的化学镇静剂[J]. 理化检验－化学分册, 2016, 52(6): 629～634
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【3】肖丽和,刘吉金,关潇滢,等.镇静安神类中成药及保健食品中非法添加化学成分的快速筛查方法研究［J］.中国当代医药, 2009,16(14):15-16.
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【7】LAURA M, FRANCESCA B, EMST K, et al.Simultaneous determination of the antipsychotic drugs levomepromazine and clozapine and their main metabolites in human plasma by a HPLC-UV method with solid-phase extraction［J］. Journal of Chromatography B, 2007,846:273-281.
【8】MARIA E, DEVASISH B. Direct injection micellar liquid chromatographic determination of benzodiazepines in serum［J］. Journal of Chromatography B, 2002,25(2):241-249.
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