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節(jié)儉之星事跡材料

第1篇:節(jié)儉之星事跡材料范文

1 引 言

熒光增白劑(Fluorescent whitening agents,F(xiàn)WA)是一種熒光染料,常被用于紙、塑料等行業(yè)的生產(chǎn)中,以提高產(chǎn)品的白度和艷度。鑒于熒光增白劑可能通過食品包裝遷移到食品,被人體吸收后會對人體造成危害,各國對熒光增白劑進(jìn)行了監(jiān)管,制定了允許用于生產(chǎn)食品接觸材料的熒光增白劑清單,如歐盟2002/72/EC[1]列出了FWA 393, FWA 184, FWA 236和FWA 368等塑料用熒光增白劑,并明確規(guī)定食品包裝紙最終產(chǎn)品的熒光增白劑的限制為“檢測不到該物質(zhì)遷移到食品中的量”[2];我國列出了FWA 393, FWA 184和FWA 236 3種塑料用熒光增白劑[3], 同時(shí)規(guī)定紙包裝產(chǎn)品“生產(chǎn)過程中不得使用熒光增白劑”[4]。因此,建立食品接觸紙包裝材料中熒光增白劑的快速定性與定量檢測方法,有利于對可能存在的違禁添加熒光增白劑行為進(jìn)行監(jiān)管。

目前,常用的熒光增白劑的檢測方法有紫外燈照射觀測法(ULO)[5]、薄層層析法(TLC)[6]、液相色譜法(HPLC)[6,7]和液相色譜串聯(lián)三重四級桿質(zhì)譜法(LCMS/MS)[7,8]等。ULO、TLC和HPLC的方法靈敏度和選擇性較差;LCMS/MS采用MRM模式檢測,靈敏度高,抗干擾能力強(qiáng),但仍受分辨率、掃描速率和模式的限制,不能滿足快速篩查的需求。高效液相色譜串聯(lián)高分辨飛行時(shí)間質(zhì)譜(LCTRIPLETOF)不僅具備了高分辨飛行時(shí)間質(zhì)譜能測得化合物及其碎片離子的分子式和精確分子量數(shù)據(jù)的特性[9~11],同時(shí)具備完全定性、同時(shí)定性定量、完全定量3種(Triple)工作流程,在LCTRIPLETOF的TOF MS觸發(fā)TOF MS/MS的模式下檢測,可以根據(jù)保留時(shí)間、一級離子質(zhì)量準(zhǔn)確度、一級離子同位素分布、二級碎片與譜庫匹配4種手段準(zhǔn)確定性,具有高分辨率、高靈敏度和高掃描速度等特點(diǎn)[12]。目前尚未見應(yīng)用LCTRIPLETOF分析熒光增白劑的報(bào)道。

本研究采用液相色譜串聯(lián)高分辨飛行時(shí)間質(zhì)譜技術(shù),以食品接觸紙包裝材料中FWA368, FWA367, FWA185, FWA184, FWA52, FWA135和FWA393(結(jié)構(gòu)圖見表1)7種熒光增白劑為研究對象,建立了7種熒光增白劑的MS/MS數(shù)據(jù)庫,并通過優(yōu)化前處理方法和色譜質(zhì)譜條件,建立了食品接觸紙質(zhì)包裝材料中熒光增白劑的定性確證及定量檢測方法。 2 實(shí)驗(yàn)部分

2.1 儀器與試劑

1 Commission Directive 2002/72/EC

2 Santos M, Batlle R, Salafranca J, Nerín C. J. Chromatogr. A, 2005, 1064: 135-141

3 GB 96852008, Hygienic Standards for Uses of Additives in Food Containers and Packaging Materials. National Standards of the People′s Republic China

食品容器、包裝材料用添加劑使用衛(wèi)生標(biāo)準(zhǔn). 中華人民共和國國家標(biāo)準(zhǔn). GB 96852008

4 The Detailed Rules for the Implementation of the Production License of Food Contact Paper Package, Containers and Other Products. Beijing: General Administration of Quality Supervision, Inspection and Quarantine of the People′s Republic of China, 2007

食品用紙包裝、容器等制品生產(chǎn)許可實(shí)施細(xì)則. 北京:國家質(zhì)量監(jiān)督檢驗(yàn)檢疫總局, 2007

5 Escabasse J Y. Ottenio D. Food Additives and Contaminants, 2002, 19: 79-92

6 XIAN YanPing, GUO XinDong, LUO HaiYing, WU YuLuan, CHEN YiGuang, LUO DongHui, WU WenHai. Chinese Journal of Chromatography, 2013, 31(2): 162-169

冼燕萍, 郭新東, 羅海英, 吳玉鑾, 陳意光, 羅東輝, 吳文海. 色譜, 2013, 31(2): 162-169

7 Chen H C, Wang S P, Ding W H. J. Chromatogr. A., 2006, 1102(12): 135-142

8 Guo X D, Xian Y P, Luo H Y, Wu Y L, Luo D H, Chen Y G, Lu Y J, Xu D. Anal. Methods, 2013, 5: 6086-6093

9 Deng X J, Yang H Q, Li J Z, Song Y, Guo D H, Luo Y, Du X N, Bo T. J. Liquid Chromatogr. Related Technol., 2011, 34: 2286-2303

10 ZHANG Feng, XU ChengBao, LAN Fang, WANG XiuJuan, YONG Wei, SUO Ran, CHU XiaoGang, DING Fei, L QuanFu. Chinese J. Anal. Chem., 2012, 40(1): 101-106

張 峰, 許成保, 藍(lán) 芳, 王秀娟, 雍 煒, 鎖 然, 儲曉剛, 丁 菲, 呂泉福. 分析化學(xué), 2012, 40(1): 101-106

11 YAN LiJuan, ZHANG Jie, PAN ChenSong, LIN LiYi, ZHANG XinYi, SHEN HeQing. Chinese J. Anal. Chem., 2013, 41(1): 31-35

嚴(yán)麗娟, 張 潔, 潘晨松, 林立毅, 張欣怡, 申河清. 分析化學(xué), 2013, 41(1): 31-35

12 LIN LiYi, YANG LiZhong, YAN LiJuan, CHEN LuPing, ZHOU Yu, XU DunMing. Journal of Food Safety and Quality, 2013, (3): 899-904

林立毅, 楊黎忠, 嚴(yán)麗娟, 陳鷺平, 周 昱, 徐敦明. 食品安全質(zhì)量檢測學(xué)報(bào), 2013, (3): 899-904

Simultaneous Determination of Seven Fluorescent Whitening

Agents in Food Contact Paper Package Materials by

High Performance Liquid Chromatography Tandem

Triple TOFHigh Resolution Mass Spectrometry

DU ZhiFeng1,2,4, XIAN YanPing1, LIU FuJian3, GUO XinDong*1, HUANG JinFeng1,

WU YuLuan1, LUO HaiYing1, WANG YongHua*4

1(Guangzhou Quality Supervision and Testing Institute, Guangzhou 510110, China)

2(AB SCIEX Asia Pacific Application Support Center, Shanghai 200233, China)

3(Guangdong Testing Institute for Product Quality Supervision, Guangzhou 510330, China)

4(College of Light Industry and Food Engineering, South China University of Technology, Guangzhou 510640, China)

Abstract A method for screening and quantitative detection of seven fluorescent whitening agents (FWAs, FWA368, FWA367, FWA185, FWA 184, FWA52, FWA135 and FWA393) in food contact paper package materials was established by high performance liquid chromatography tandem triple TOF high resolution mass spectrometry (LCTriple TOF MS). The paper samples were extracted with chloroform under ultrasonication, concentrated, separated in a C18 column (100 mm× 2.1 mm i. d., 2.6 μm) by gradient elution using methanol and 0.1% formic acid in water as mobile phase, and detected in positive ESI and TOFMS IDA MS/MS mode. The qualitative analysis of seven FWAs was confirmed by synergistic effect of retention time, mass accuracy of precursor, isotope distribution of the precursor, and library search. The analytes were quantified by peak areas of the TOFMS extracted ions. The results indicated that, all of the seven FWAs presented favorable mass accuracy less than 3×10Symbolm@@ 6, good linearity in the concentration of 4-400 μg/L with the correlation coefficients larger than 0.996, low instrument detection limits (S/N=3) of 1.0-5.0 μg/kg, appropriate recoveries ranged from 81.2% to 98.9% at three spiked levels, and satisfactory RSD (n=6) of 5.2%-9.1%. 13 samples were tested using the method and one sample was found FWA 184 with concentration of 287 μg/kg. The method is efficient and accurate, and is suitable for analysis of the seven FWAs in food contact paper package materials.