液相色谱高分辨飞行时间质谱法测定食品接触纸包装材料中的7种荧光增白剂
杜志峰等
摘 要 建立了食品接触纸包装材料中7种荧光增白剂
1 引 言
荧光增白剂(Fluorescent whitening agents,FWA)是一种荧光染料,常被用于纸、塑料等行业的生产中,以提高产品的白度和艳度。鉴于荧光增白剂可能通过食品包装迁移到食品,被人体吸收后会对人体造成危害,各国对荧光增白剂进行了监管,制定了允许用于生产食品接触材料的荧光增白剂清单,如欧盟2002/72/EC[1]列出了FWA 393, FWA 184, FWA 236和FWA 368等塑料用荧光增白剂,并明确规定食品包装纸最终产品的荧光增白剂的限制为“检测不到该物质迁移到食品中的量”[2];我国列出了FWA 393, FWA 184和FWA 236 3种塑料用荧光增白剂[3], 同时规定纸包装产品“生产过程中不得使用荧光增白剂”[4]。因此,建立食品接触纸包装材料中荧光增白剂的快速定性与定量检测方法,有利于对可能存在的违禁添加荧光增白剂行为进行监管。
目前,常用的荧光增白剂的检测方法有紫外灯照射观测法(ULO)[5]、薄层层析法(TLC)[6]、液相色谱法(HPLC)[6,7]和液相色谱串联三重四级杆质谱法(LCMS/MS)[7,8]等。ULO、TLC和HPLC的方法灵敏度和选择性较差;LCMS/MS采用MRM模式检测,灵敏度高,抗干扰能力强,但仍受分辨率、扫描速率和模式的限制,不能满足快速筛查的需求。高效液相色谱串联高分辨飞行时间质谱(LCTRIPLETOF)不仅具备了高分辨飞行时间质谱能测得化合物及其碎片离子的分子式和精确分子量数据的特性[9~11],同时具备完全定性、同时定性定量、完全定量3种(Triple)工作流程,在LCTRIPLETOF的TOF MS触发TOF MS/MS的模式下检测,可以根据保留时间、一级离子质量准确度、一级离子同位素分布、二级碎片与谱库匹配4种手段准确定性,具有高分辨率、高灵敏度和高扫描速度等特点[12]。目前尚未见应用LCTRIPLETOF分析荧光增白剂的报道。
本研究采用液相色谱串联高分辨飞行时间质谱技术,以食品接触纸包装材料中FWA368, FWA367, FWA185, FWA184, FWA52, FWA135和FWA393(结构图见表1)7种荧光增白剂为研究对象,建立了7种荧光增白剂的MS/MS数据库,并通过优化前处理方法和色谱质谱条件,建立了食品接触纸质包装材料中荧光增白剂的定性确证及定量检测方法。 2 实验部分
2.1 仪器与试剂
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、包装材料用添加剂使用卫生标准. 中华人民共和国国家标准. 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
食品用纸包装、容器等制品生产许可实施细则. 北京:国家质量监督检验检疫总局, 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, 郭新东, 罗海英, 吴玉銮, 陈意光, 罗东辉, 吴文海. 色谱, 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
张 峰, 许成保, 蓝 芳, 王秀娟, 雍 炜, 锁 然, 储晓刚, 丁 菲, 吕泉福. 分析化学, 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
严丽娟, 张 洁, 潘晨松, 林立毅, 张欣怡, 申河清. 分析化学, 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, 杨黎忠, 严丽娟, 陈鹭平, 周 昱, 徐敦明. 食品安全质量检测学报, 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.
Keywords High performance liquid chromatography tandem triple time of flighthigh resolution mass spectrometry; Fluorescent whitening agents; Food contact paper package materials
(Received 27 August 2013; accepted 31 December 2013)
张 峰, 许成保, 蓝 芳, 王秀娟, 雍 炜, 锁 然, 储晓刚, 丁 菲, 吕泉福. 分析化学, 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
严丽娟, 张 洁, 潘晨松, 林立毅, 张欣怡, 申河清. 分析化学, 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, 杨黎忠, 严丽娟, 陈鹭平, 周 昱, 徐敦明. 食品安全质量检测学报, 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.
Keywords High performance liquid chromatography tandem triple time of flighthigh resolution mass spectrometry; Fluorescent whitening agents; Food contact paper package materials
(Received 27 August 2013; accepted 31 December 2013)
张 峰, 许成保, 蓝 芳, 王秀娟, 雍 炜, 锁 然, 储晓刚, 丁 菲, 吕泉福. 分析化学, 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
严丽娟, 张 洁, 潘晨松, 林立毅, 张欣怡, 申河清. 分析化学, 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, 杨黎忠, 严丽娟, 陈鹭平, 周 昱, 徐敦明. 食品安全质量检测学报, 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.
Keywords High performance liquid chromatography tandem triple time of flighthigh resolution mass spectrometry; Fluorescent whitening agents; Food contact paper package materials
(Received 27 August 2013; accepted 31 December 2013)
摘 要 建立了食品接触纸包装材料中7种荧光增白剂
1 引 言
荧光增白剂(Fluorescent whitening agents,FWA)是一种荧光染料,常被用于纸、塑料等行业的生产中,以提高产品的白度和艳度。鉴于荧光增白剂可能通过食品包装迁移到食品,被人体吸收后会对人体造成危害,各国对荧光增白剂进行了监管,制定了允许用于生产食品接触材料的荧光增白剂清单,如欧盟2002/72/EC[1]列出了FWA 393, FWA 184, FWA 236和FWA 368等塑料用荧光增白剂,并明确规定食品包装纸最终产品的荧光增白剂的限制为“检测不到该物质迁移到食品中的量”[2];我国列出了FWA 393, FWA 184和FWA 236 3种塑料用荧光增白剂[3], 同时规定纸包装产品“生产过程中不得使用荧光增白剂”[4]。因此,建立食品接触纸包装材料中荧光增白剂的快速定性与定量检测方法,有利于对可能存在的违禁添加荧光增白剂行为进行监管。
目前,常用的荧光增白剂的检测方法有紫外灯照射观测法(ULO)[5]、薄层层析法(TLC)[6]、液相色谱法(HPLC)[6,7]和液相色谱串联三重四级杆质谱法(LCMS/MS)[7,8]等。ULO、TLC和HPLC的方法灵敏度和选择性较差;LCMS/MS采用MRM模式检测,灵敏度高,抗干扰能力强,但仍受分辨率、扫描速率和模式的限制,不能满足快速筛查的需求。高效液相色谱串联高分辨飞行时间质谱(LCTRIPLETOF)不仅具备了高分辨飞行时间质谱能测得化合物及其碎片离子的分子式和精确分子量数据的特性[9~11],同时具备完全定性、同时定性定量、完全定量3种(Triple)工作流程,在LCTRIPLETOF的TOF MS触发TOF MS/MS的模式下检测,可以根据保留时间、一级离子质量准确度、一级离子同位素分布、二级碎片与谱库匹配4种手段准确定性,具有高分辨率、高灵敏度和高扫描速度等特点[12]。目前尚未见应用LCTRIPLETOF分析荧光增白剂的报道。
本研究采用液相色谱串联高分辨飞行时间质谱技术,以食品接触纸包装材料中FWA368, FWA367, FWA185, FWA184, FWA52, FWA135和FWA393(结构图见表1)7种荧光增白剂为研究对象,建立了7种荧光增白剂的MS/MS数据库,并通过优化前处理方法和色谱质谱条件,建立了食品接触纸质包装材料中荧光增白剂的定性确证及定量检测方法。 2 实验部分
2.1 仪器与试剂
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、包装材料用添加剂使用卫生标准. 中华人民共和国国家标准. 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
食品用纸包装、容器等制品生产许可实施细则. 北京:国家质量监督检验检疫总局, 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, 郭新东, 罗海英, 吴玉銮, 陈意光, 罗东辉, 吴文海. 色谱, 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
张 峰, 许成保, 蓝 芳, 王秀娟, 雍 炜, 锁 然, 储晓刚, 丁 菲, 吕泉福. 分析化学, 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
严丽娟, 张 洁, 潘晨松, 林立毅, 张欣怡, 申河清. 分析化学, 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, 杨黎忠, 严丽娟, 陈鹭平, 周 昱, 徐敦明. 食品安全质量检测学报, 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.
Keywords High performance liquid chromatography tandem triple time of flighthigh resolution mass spectrometry; Fluorescent whitening agents; Food contact paper package materials
(Received 27 August 2013; accepted 31 December 2013)
张 峰, 许成保, 蓝 芳, 王秀娟, 雍 炜, 锁 然, 储晓刚, 丁 菲, 吕泉福. 分析化学, 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
严丽娟, 张 洁, 潘晨松, 林立毅, 张欣怡, 申河清. 分析化学, 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, 杨黎忠, 严丽娟, 陈鹭平, 周 昱, 徐敦明. 食品安全质量检测学报, 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.
Keywords High performance liquid chromatography tandem triple time of flighthigh resolution mass spectrometry; Fluorescent whitening agents; Food contact paper package materials
(Received 27 August 2013; accepted 31 December 2013)
张 峰, 许成保, 蓝 芳, 王秀娟, 雍 炜, 锁 然, 储晓刚, 丁 菲, 吕泉福. 分析化学, 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
严丽娟, 张 洁, 潘晨松, 林立毅, 张欣怡, 申河清. 分析化学, 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, 杨黎忠, 严丽娟, 陈鹭平, 周 昱, 徐敦明. 食品安全质量检测学报, 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.
Keywords High performance liquid chromatography tandem triple time of flighthigh resolution mass spectrometry; Fluorescent whitening agents; Food contact paper package materials
(Received 27 August 2013; accepted 31 December 2013)