•  
  •  
 

Authors

HAN Zhi, Hubei Provincial Institute for Food Supervision and Test, Wuhan, Hubei 430070, China; Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Wuhan, Hubei 430070, China
GONG Lei, Hubei Provincial Institute for Food Supervision and Test, Wuhan, Hubei 430070, China; Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Wuhan, Hubei 430070, China
WANG Huixia, Hubei Provincial Institute for Food Supervision and Test, Wuhan, Hubei 430070, China; Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Wuhan, Hubei 430070, China
ZHU Xiaoling, Hubei Provincial Institute for Food Supervision and Test, Wuhan, Hubei 430070, China; Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Wuhan, Hubei 430070, China
WU Wanqin, Hubei Provincial Institute for Food Supervision and Test, Wuhan, Hubei 430070, China; Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Wuhan, Hubei 430070, China
LIU Guojiao, Hubei Provincial Institute for Food Supervision and Test, Wuhan, Hubei 430070, China; Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Wuhan, Hubei 430070, China
WANG Bin, Hubei Provincial Institute for Food Supervision and Test, Wuhan, Hubei 430070, China; Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test, Wuhan, Hubei 430070, China

Abstract

A high-throughput qualitative screening and quantita-tive method of ultra-high performance liquid chromatography combined with orbitrap mass spectrometry(UPLC-Orbitrap-MS) was developed to determine 73 kinds of chemicals illegally added in the healthy foods. The samples were extracted with methanol using ultrasonic extraction. The separation was eluted by gradient on a Waters Acquity UPLC HSS T3 column (100 mm×2.1 mm, 1.8 μm), with a mobile phase consisting of water (0.1% formic acid) and acetonitrile in both positive and negative mode. The data were acquired via full-scan data-dependent MS/MS (full scan-ddMS2). The qualitative analyses of the compounds were performed through the database established by Trace Finder software, and the quantitative detection were undertaken through the area of precursor ions. The results showed that each target had good linearity in its own concentration range, and the correlation coefficients were higher than 0.99. The limits of determination (LODs) were between 2~20 μg/kg, and the limits of quantification (LOQs) were between 6~60 μg/kg. The recoveries of the proposed method were in range of 72.2%~117.5% at spiked levels of 100, 200, and 1 000 μg/kg with deviations (RSDs) between 2.3%~6.8%. It could be concluded that the high-throughput, qualitative and quantitative method reported in this study was useful for the determination of illicit drugs in functional foods.

Publication Date

7-28-2019

First Page

74

Last Page

79,116

DOI

10.13652/j.issn.1003-5788.2019.07.013

References

[1] 张雪艳, 王素珍. 保健食品市场乱象成因分析及对策[J]. 中国食品药品监管, 2018(8): 49-53.
[2] 曹进, 黄湘鹭, 张庆生, 等. 食品和保健食品中非法添加物筛查策略的建立[J]. 食品科学, 2014, 35(19): 302-306.
[3] 食品药品监管总局办公厅. 总局办公厅关于印发国家食品安全监督抽检实施细则(2018年版)的通知. (2018-01-18)[2019-03-01]. http://samr.cfda.gov.cn/WS01/CL1605/223270.html.
[4] 李静辉, 刘吉成, 马德志, 等. 薄层色谱—表面增强拉曼光谱法快速检测改善睡眠类保健食品的主要成分及其光谱表征[J]. 中国食品卫生杂志, 2018, 30(4): 376-382.
[5] 李静辉, 程闹闹, 刘吉成, 等. TLC-SERS法快速检测改善睡眠类保健食品中四种化学成分[J]. 光谱学与光谱分析, 2018, 38(4): 1 122-1 128.
[6] 许凤, 李晓雪, 李莉, 等. 基于薄层色谱原位富集显微拉曼光谱法快速检测降压保健食品中非法添加的3种西药[J]. 高等学校化学学报, 2018, 39(6): 1 172-1 177.
[7] 李瑞婷, 陆建超, 王弘, 等. 直接竞争酶联免疫吸附法用于糖浆类保健食品中西地那非检测的研究[J]. 食品工业科技, 2014, 35(24): 84-88, 95.
[8] VTZSLAV M, ZNALEZIONA J, JIROVSKY D, et al. Determination of antihyperglycemic drugs in nanomolar concentration levels by micellarelectrokinetic chromatography with non-ionic surfactant[J]. Journal of Chromatography A, 2009, 1 216(20): 4 492-4 498.
[9] 林芳, 李涛, 王一欣, 等. 超高效液相色谱法同时测定降糖类保健食品中非法添加的13种化学药物[J]. 食品科学, 2016, 37(18): 178-184.
[10] 林芳, 李涛, 耿庆光, 等. 超高效液相色谱—二极管阵列检测器法快速测定保健食品中违法添加的14种性功能药物[J]. 食品科学, 2014, 35(4): 163-169.
[11] 陈毓芳, 林海丹, 吴宏中, 等. 高效液相色谱法同时测定保健食品中11种功效成分[J]. 食品科学, 2015, 36(8): 244-249.
[12] KROGH M, GREFSLIE H, RASMUSSEN K E. Solvent-modified solid-phase microextraction for the determination of diazepam in human plasma samples by capillary gas chromatography[J]. Journal of Chromatography B Biomedical Sciences & Applications, 1997, 689(2): 357-364.
[13] GUNNAR T, ARINIEMI K, LILLSUNDE P. Determina-tion of 14 benzodiazepines and hydroxy metabolites, zaleplon and zolpidem as tert-butyldimethylsilyl derivatives compared with other common silylating reagents in whole blood by gas chromatography-mass spectrometry[J]. Journal of Chromatography B, 2005, 818(2): 175-189.
[14] 李晓蕾, 陈军, 杨朝芬, 等. 超高效液相色谱—串联质谱法检测辅助降血脂保健食品中6种非法添加化学药物[J]. 食品科学, 2018, 39(18): 320-325.
[15] CHEN Y, ZHAO L, LU F, et al. Determination of synthetic drugs used to adulterate botanical dietary supplements using QTRAP LC-MS/MS[J]. Food Additives and Contaminants: Part A, 2009, 26(5): 595-603.
[16] KIM J Y, PARK H J, KIM J W, et al. Development and validation of UPLC and LC-MS/MS methods for the simultaneous determination of anti-obesity drugs in foods and dietary supplements[J]. Archives of Pharmacal Research, 2016, 39(1): 103-114.
[17] 康宁, 高媛惠, 高利珍. 高效液相色谱—串联飞行时间质谱法检测安神类保健食品中非法添加物[J]. 食品与机械, 2018, 34(10): 49-54.
[18] 宫旭, 芦丽, 冯有龙, 等. HPLC-IT-TOF-MS快速检测减肥、降脂、降糖类保健食品中非法添加的25种化学药品[J]. 中国药师, 2018, 21(8): 1 463-1 468.
[19] 姜春来, 邢俊波, 靳守东. HPLC-Q-TOF法测定降糖类中成药及保健食品中14种非法添加药物[J]. 解放军药学学报, 2016, 32(6): 514-517.
[20] 于泓, 胡青, 张甦, 等. 超高效液相色谱—四级杆—飞行时间串联质谱法检测中药及保健食品中21种非法添加的降脂类药物[J]. 食品安全质量检测学报, 2016, 7(7): 2 704-2 709.
[21] MAKAROV A. Electrostatic axially harmonic orbital trapping: A high-performance technique of mass analysis[J]. Analytical Chemistry, 2000, 72(6): 1 156-1 162.
[22] 张晓光, 李强, 孙磊, 等. 超高效液相色谱—静电场轨道阱高分辨质谱快速筛查保健品中23种非法添加西药成分[J]. 食品科学, 2015, 36(14): 187-191.
[23] 刘芸, 丁涛, 廖雪晴, 等. 高效液相色谱—四极杆/静电场轨道阱高分辨率质谱法快速筛查中成药和保健食品中非法添加的42种化学药物[J]. 分析化学, 2016, 44(3): 423-429.
[24] 食品药品监管总局. 总局关于发布《保健食品中75种非法添加化学药物的检测》等3项食品补充检验方法的公告(2017年第138号). (2017-11-17) [2019-03-01]. http://samr.cfda.gov.cn/WS01/CL0087/217375.html.
[25] 市场监管总局. 市场监管总局关于发布《食品中那非类物质的测定》食品补充检验方法的公告. (2018-07-02)[2019-03-01]. http://samr.saic.gov.cn/gg/201807/t20180704_274876.html.

Share

COinS
 
 

To view the content in your browser, please download Adobe Reader or, alternately,
you may Download the file to your hard drive.

NOTE: The latest versions of Adobe Reader do not support viewing PDF files within Firefox on Mac OS and if you are using a modern (Intel) Mac, there is no official plugin for viewing PDF files within the browser window.