Microsoft Word 何欢-二校

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1 5 9 Vol. 5 No Journal of Food Safety and Quality Sep., 2014 何欢 1, 王静文 1, 李琼 2, 罗中玉 2, 曹进 1*, 王钢力 1, 张庆生 1 (1., ; 2., ) 摘要 : 目的方法 39 (IMS), 39 IMS,,, 结果 39, 10%, 5% 结论 IMS,, 关键词 : ; ; Identification of illegally added chemicals in health foods for weight loss by ion mobility spectrometry HE Huan 1, WANG Jing-Wen 1, LI Qiong 2, LUO Zhong-Yu 2, CAO Jin 1*, WANG Gang-Li 1, ZHANG Qing-Sheng 1 (1. National Institutes for Food and Drug Control, Beijing , China; 2. Chinese Food Industry Investment Guarantee Corporation, Beijing , China) ABSTRACT: Objective To establish a new method for screening chemicals illegally added in health foods. Methods Totally 39 kinds of common weight loss drugs were detected by ion mobility spectrometry (IMS) to establish IMS test database of 39 potential illegal addition chemicals. The sample was dissolved with ethanol, then dropped in test paper with the supernatant, after that detected directly. Ion mobility spectrometry was used to build a screening method for illegal addition in weight loss health foods. Results Totally 39 potential illegal addition chemicals were detected by IMS. The false positive ratio was below 10% as well as false negative ratio below 5%. Conclusion IMS can be used to screen the drugs illegal additions in healthy foods. It has relatively high screening efficiency, and can be regarded as a rapid and reliable technique in healthy foods supervision and inspection. KEY WORDS: health foods; ion mobility spectrometry; illegal addition 1 引言,,,,,,, 基金项目 : (2012BAK08B02) Fund: Supported by National Key Technology R&D Program (2012BAK08B02) * 通讯作者 :,, caojin@nifdc.org.cn *Corresponding author: CAO Jin, Associate Researcher, National Institutes for Food and Drug Control, No.2, Tiantan Xili, Dongcheng District, Beijing , China. caojin@nifdc.org.cn

2 2658 5,, [1] : (1),,,,,, ; [2],,, FDA(Food and Drug Administration) 1997 (2),,,,, (3),, 1997 FDA (ion mobility spectrometry, IMS) [3-5] IMS ( ng pg ), IMS [6-9],,, [10-14],,,,,,, [15] [16,17],, IMS,, 2 材料与方法 2.1 材料及设备 TR2000( );, ; 2.2 IMS 检测条件 63 Ni,,,, 1 表 1 IMS 检测参数 Table 1 Detection parameters of IMS L/min L/min 样品前处理方法 50 ml (,, ), 50 ml, 1 min, 15 min, 10 µl, 3 结果与分析种减肥类药物的 IMS 检测数据库, 39 IMS, 1,, 2,, 种阳性减肥类保健食品的 IMS 快速检测, 20 IMS, 多种药品的混合快筛, IMS, 4

3 9, : 2659 表 2 39 种减肥药物的 IMS 检测结果 (n=20) Table 2 IMS testing results of 39 kinds of anti-obesity drugs(n=20) (ms) (ng/μl) N N-N : : : : : : : : : : :

4 Table 3 表 3 LC-MS 与 IMS 分析结果的比较 (n=5) Comparison of LC-MS and IMS analysis results (n=5) LC-MS IMS 表 4 药物混合物的 IMS 筛查结果 (n=10) Table 4 IMS screening results of drug mixtures (n=10) IMS

5 9, : 讨论 4.1 检测条件的选择,,,,, 2, 1,, 3, 4,,, ng~μg, ;, RSD 20%,, ; 50%~120%, 100%~120%, 4.2 筛查方法的检出限及运行稳定性,,, 39, IMS,, IMS,,, 5%, 10%,, 3%, 4.3 减肥类药物的 IMS 数据库的建立 39, ng/μl ; ng/μl ; ng/μl 4.4 实际样品测定 IMS 4 7, IMS 4 6, 4.5 结论,,, IMS,,,, 参考文献 [1],,. 7 [J]., 2011, 39(11): Li Y, Xue F, Wang Y, et al. Simultaneous Determination of Seven Adulterants in Slimming Functional Foods by High Performance Capillary Electrophoresis[J]. Chin J Anal Chem, 2011,39(11): [2],,,. 8 [J]., 2004, 32(3): Wang S, Mi JB, Chang WB, et al. Analysis of 8 Synthetic Anorexics in Adulterated Weight-reducing Tonic[J]. Chin J Anal Chem, 2004, 32(3): [3] Baumbach JI, Eiceman GA. Ion mobility spectrometry: arriving on site and moving beyond a low profile[j]. Appl Spectrosc, 2001, (53): 338A 355A. [4],,,. [J]., 2014, 35(2): Liu L, Hua R, Wang J, et al. Research Progress of Ionization Technologies for Ion Mobility Spectrometry [J]. J Chin Mass Spectr Soc, 2014, 35(2): [5],,. [J]., 2005, 17(3): Xu F, Wang HL, Guan YF. Progress in ion mobility spectrometry[j]. Prog Chem, 2005, 17(3): [6] Dussy FE, Berchtold C, Briellmann TA, et al. Validation of an ion mobility spectrometry (IMS) method for the detection of heroin and cocaine on incriminated material[j]. Forensic Sci Int, 2008, 177(2-3): [7] Bell SE, Ewing RG, Eiceman GA, et al. Atmospheric pressure

6 chemical ionization of alkanes, alkenes, and cycloalkanes[j]. J Am Soc Mass Spectr, 1994, 5 (3): [8],,,. [J]., 2014,42(2): Peng LY, Wang WG, Wang X, et al. Rapid Screening of Trace Phthalate Estersin-Wine Using Ion Mobility Spectrometry[J]. Chin J Anal Chem, 2014, 42(2): [9] Armenta S, Alcala M, Blanco M. A review of recent, unconventional applications of ion mobility spectrometry (IMS)[J]. Anal Chim Acta, 2011, 703(2): [10] Crawford CL, Hill HH. Evaluation of false positive responses by mass spectrometry and ion mobility spectrometry for the detection of trace explosives in complex samples[j]. Anal Chim Acta, 2013, (795): [11] Eiceman GA, Karpas Z, Hill HH, et al. Ion Mobility Spectrometry[M]. CRC Press, [12],,,. [J]., 2014, 42(4): Li LF, Wang TS, Han K, et al. Rapid Identification of Illegally Addition in Traditional Chinese Antidiabetic Medicine by Field Asymmetric Ion Mobility Spectrometric Technique[J]. Chin J Anal Chem, 2014, 42(4): [13] Connie MG, John CR, John FK, et al. Detection of undeclared erectile dysfunction drugs and analogues in dietary supplements by ion mobility spectrometry [J]. J Pharm Biomed Anal, 2009, 49(3): [14] Armenta S, Alcala M, Blanco M, et al. Ion mobility spectrometry for the simultaneous determination of diacetyl midecamycin and detergents in cleaning validation [J]. J Pharm Biomed Anal, 2013, 83: [15],,,. [J]., 2006, 34(12): Jia J, Guo HY, Gao XG, et al. Effects of Drift Tube Temperature on Ion Mobility Spectra [J]. Chin J Anal Chem, 2006, 34(12): [16],,,. [J]., 2013, 26(11): 4 7. Lin L, Niu YW, Ma J, et al. Research progress of applying ion mobility spectrometry in food safety rapid detection [J]. Cereals Oils, 2013, 26(11): 4 7. [17],,,. [J]., 2011, 30(4): Wang JF, Zhang ZX, Du ZX, et al. Detection of malathion and dichlorovos in cherry tomatoes using a hand-held ion mobility spectrometer [J]. Chin J Anal Lab, 2011, 30(4): 作者简介 ( 责任编辑 : 张宏梁 ) 何欢, 研究生, 助理研究员, 主要研究方向为分析化学 hehuan_725@aliyun.com 曹进, 副研究员, 主要研究方向为分析化学 caojin@nifdc.org.cn

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