固相萃取-高效液相色谱法同时测定饮水纸杯中荧光增白剂OB和CBS-127的含量
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摘要
利用固相萃取-高效液相色谱法同时测定饮水纸杯中荧光增白剂2,5-双-(5-叔丁基-2-苯并恶唑基)噻吩(OB)和4,4-双(2-甲氧基苯乙烯基)联苯(CBS-127)的含量,样品经二氯甲烷超声提取,CN固相萃取柱纯化后,以V(乙腈)∶V(甲醇)∶V(水)(20∶75∶5)为流动相,高效液相色谱-荧光检测器测定。结果表明:荧光增白剂OB和CBS-127可以得到较好的分离检测,混合溶液在0.01~1mg·L-1范围内线性关系良好,OB的线性关系为Y=30.938 X+1.396 8,相关系数为0.999 6,检出限为1.5×10~(-3) mg·kg~(-1),相对标准偏差为1.24%;CBS-127的线性关系为Y=62.271 X+1.589 8,相关系数为0.999 8,检出限为3×10-3 mg·kg~(-1),相对标准偏差为1.33%。实际样品的加标平均回收率为79%~92%,该方法样品处理简单、精密度好,适用于同时测定饮水纸杯中OB和CBS-127。
Simultaneous determination the content of the paper drinking water cup of fluorescent whitening agent 2,5-di(5-tert-butylbenzoxazol-2-yl)thiophene(OB)and 4,4′-bis(2-methoxystyryl)-1,1′-biphenyl(CBS-127)with solid phase extraction method using high performance liquid chromatography(HPLC),the samples were ultrasound extracted by dichloromethane,purified by CN solid phase extraction,V(acetonitrile)∶V(methanol)∶V(water)=20∶75∶5as mobile phase,HPLC fluorescence detector determination,the results shows that:the fluorescent whitening agent OB and CBS-127 can be isolated well,the mixed solution at range of 0.01—1mg·L-1 have a good linear relationship,the fluorescent whitening agent OB was Y=30.938 X+1.396 8,the correlation coefficient was 0.999 6,the detection limit is1.5×10-3 mg·kg~(-1),the relative standard deviation was 1.24%,the linear relationship of the fluorescent whitening agent CBS-127 was Y=62.271 X+1.589 8,the correlation coefficient was 0.999 8,the detection limit is 3×10-3 mg·kg~(-1),the relative standard deviation is1.33%.average spiked recovery rate was 79%—92%.The sample treatment is simple,precision,it is suitable for simultaneous determination of drinking cups of fluorescent whitening agents in OB and CBS-127.
Simultaneous determination the content of the paper drinking water cup of fluorescent whitening agent 2,5-di(5-tert-butylbenzoxazol-2-yl)thiophene(OB)and 4,4′-bis(2-methoxystyryl)-1,1′-biphenyl(CBS-127)with solid phase extraction method using high performance liquid chromatography(HPLC),the samples were ultrasound extracted by dichloromethane,purified by CN solid phase extraction,V(acetonitrile)∶V(methanol)∶V(water)=20∶75∶5as mobile phase,HPLC fluorescence detector determination,the results shows that:the fluorescent whitening agent OB and CBS-127 can be isolated well,the mixed solution at range of 0.01—1mg·L-1 have a good linear relationship,the fluorescent whitening agent OB was Y=30.938 X+1.396 8,the correlation coefficient was 0.999 6,the detection limit is1.5×10-3 mg·kg~(-1),the relative standard deviation was 1.24%,the linear relationship of the fluorescent whitening agent CBS-127 was Y=62.271 X+1.589 8,the correlation coefficient was 0.999 8,the detection limit is 3×10-3 mg·kg~(-1),the relative standard deviation is1.33%.average spiked recovery rate was 79%—92%.The sample treatment is simple,precision,it is suitable for simultaneous determination of drinking cups of fluorescent whitening agents in OB and CBS-127.
引文
[1]焦艳娜,丁利,朱绍华.高效液相色谱-荧光检测法测定食品接触材料塑料制品中荧光增白剂[J].色谱,2013,31(1):83-87.JIAO Yanna,DING Li,ZHU Shaohua.Determination of fluorescent whitening agent in plastic products of food contact materials by high performance liquid chromatography fluorescence detection[J].Chromatography,2013,31(1):83-87.
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[8]赵雪萍,郑晓菊,许泳吉.固相萃取-高效液相色谱法测定清麴酱中的多胺[J].青岛科技大学学报(自然科学版),2012,33(增):18-21.ZHAO Xueping,ZHENG Xiaoju,XU Yongji.Determination of polyamines in Korea chungkukjang in solid phase extraction and high performance liquid chromatography[J].Journal of Qingdao University of Science and Technology(Natural Science Edition),2012,33(Sup):18-21.
[9]冼燕萍,郭新东,罗海英,等.固相萃取-超高效液相色谱分离测定洗涤用品中4种荧光增白剂[J].色谱,2013,31(2):162-169.XIAN Yanping,GUO Xindong,LUO Haiying,et al.Solid phase extraction and ultra-performance liquid chromatography separation and determination of 4kinds of fluorescent whitening agents for washing products[J].Chromatograph,2013,31(2):162-169.
[10]刘荣琴,高磊红,王未肖,等.紫外分光光度法测定食品包装用纸中的荧光增白剂[J].广州化工,2013,41(15):135-137.LIU Rongqin,GAO Leihong,WANG Weixiao,et al.Determination of fluorescent whitening agent in food packaging paper by ultraviolet spectrophotometry[J].Guangzhou Chemical,2013,41(15):135-137.
[11]罗冠中,刘祥,汪晓冬,等.荧光分光光度法测定生活用纸制品中的荧光增白剂[J].中国测试,2009,35(4):68-71.LUO Guanzhong,LIU Xiang,WANG Xiaodong,et al.Fluorospectrophotometry determination of fluorescent whitening agent in life paper products[J].China Test,2009,35(4):68-71.
[12]沈华丽,沈淑英.高效液相色谱外标法测定荧光增白剂ER-1含量[J].印染助剂,2011,28:53-55.SHEN Huali,SHEN Shuying.Determination of fluorescent whitening agent ER-1by high performance liquid of chromatography[J].Dyeing and Printing Auxiliary,2011,28:53-55.
[13]马会娟,马强,白桦,等.洗涤用品中5种荧光增白剂的高效液相色谱法检测及质谱确证[J].分析试验室,2014,33(5):569-573.MA Huijuan,MA Qiang,BAI Hua,et al.Determination of 5kinds of fluorescent whitening agents in washing products and mass spectra[J].Analysis Laboratory,2014,33(5):569-573.
[14]庞月红,巩宗爱,张明如,等.食品包装荧光增白剂检测方法研究进展[J].食品工业科技,2013,34(18):387-390.PANG Yuehong,GONG Zongai,ZHANG Mingru,et al.Research progress of fluorescent whitening agent for food packaging[J].Food Industry Science and Technology,2013,34(18):387-390.
[2]JEONG S K,DO H K.Determination of fluorescent whitening agents in paper matericals by ion-pair reversed-phase high-performance liquid chromatography[J].Bulletin of the Koreon Chemical Society,2012,33(12):3971-3976.
[3]SHU W C,DING W H.Determination of fluorescent whitening agents in laundry detergents and surface waters by solid-phase extraction and ion-pair high-performance liquid chromatography[J].Chromatography A,2005,1088:218-223.
[4]张贵民.荧光增白剂及其安全性和环保性[J].中国洗涤品工业,2011(6):43-47.ZHANG Guimin.Fluorescent whitening agent and its safety and environmental protection[J].China Washing Product Industry,2011(6):43-47.
[5]CHEN H C,DING W H.Hot-water and solid-phase extraction of fluorescent whitening agents in paper materials and infant clothes followed by unequivocal determination with ion-pair chromatography-tandem mass spectrometry[J].Chromatography A,2006,1108:202-207.
[6]应玲,许峰,金发根,等.高效液相色谱法测定荧光增白剂OB[J].分析测试技术与仪器,1995,1(2):15-18.YING Ling,XU Feng,JIN Fagen,et al.Determination of fluorescent whitening agent by high performance liquid chromatography[J].Analytical Testing Techniques and Instruments,1995,1(2):15-18.
[7]李自红,魏悦,范毅,等.HPLC法测定荧光增白剂CBS-127的含量[J].河南科学,2013,31(1):46-48.LI Zihong,WEI Yue,FAN Yi,et al.Determination of the content of fluorescent whitening agent CBS-127 by HPLC[J].Henan Science,2013,31(1):46-48.
[8]赵雪萍,郑晓菊,许泳吉.固相萃取-高效液相色谱法测定清麴酱中的多胺[J].青岛科技大学学报(自然科学版),2012,33(增):18-21.ZHAO Xueping,ZHENG Xiaoju,XU Yongji.Determination of polyamines in Korea chungkukjang in solid phase extraction and high performance liquid chromatography[J].Journal of Qingdao University of Science and Technology(Natural Science Edition),2012,33(Sup):18-21.
[9]冼燕萍,郭新东,罗海英,等.固相萃取-超高效液相色谱分离测定洗涤用品中4种荧光增白剂[J].色谱,2013,31(2):162-169.XIAN Yanping,GUO Xindong,LUO Haiying,et al.Solid phase extraction and ultra-performance liquid chromatography separation and determination of 4kinds of fluorescent whitening agents for washing products[J].Chromatograph,2013,31(2):162-169.
[10]刘荣琴,高磊红,王未肖,等.紫外分光光度法测定食品包装用纸中的荧光增白剂[J].广州化工,2013,41(15):135-137.LIU Rongqin,GAO Leihong,WANG Weixiao,et al.Determination of fluorescent whitening agent in food packaging paper by ultraviolet spectrophotometry[J].Guangzhou Chemical,2013,41(15):135-137.
[11]罗冠中,刘祥,汪晓冬,等.荧光分光光度法测定生活用纸制品中的荧光增白剂[J].中国测试,2009,35(4):68-71.LUO Guanzhong,LIU Xiang,WANG Xiaodong,et al.Fluorospectrophotometry determination of fluorescent whitening agent in life paper products[J].China Test,2009,35(4):68-71.
[12]沈华丽,沈淑英.高效液相色谱外标法测定荧光增白剂ER-1含量[J].印染助剂,2011,28:53-55.SHEN Huali,SHEN Shuying.Determination of fluorescent whitening agent ER-1by high performance liquid of chromatography[J].Dyeing and Printing Auxiliary,2011,28:53-55.
[13]马会娟,马强,白桦,等.洗涤用品中5种荧光增白剂的高效液相色谱法检测及质谱确证[J].分析试验室,2014,33(5):569-573.MA Huijuan,MA Qiang,BAI Hua,et al.Determination of 5kinds of fluorescent whitening agents in washing products and mass spectra[J].Analysis Laboratory,2014,33(5):569-573.
[14]庞月红,巩宗爱,张明如,等.食品包装荧光增白剂检测方法研究进展[J].食品工业科技,2013,34(18):387-390.PANG Yuehong,GONG Zongai,ZHANG Mingru,et al.Research progress of fluorescent whitening agent for food packaging[J].Food Industry Science and Technology,2013,34(18):387-390.