离子色谱串联质谱法测定婴幼儿配方奶粉中氯酸盐和高氯酸盐
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摘要
目的建立离子色谱串联质谱法(ion chromatography tandem mass spectrometry, IC-MS/MS)检测婴幼儿配方奶粉中氯酸盐和高氯酸盐的分析方法。方法样品经提取、净化除去蛋白质及脂类物质后,采用离子色谱法分离,电喷雾串联质谱法测定,并采用氯酸盐-~(18)O_3和高氯酸盐-~(18)O_4作为同位素内标物质进行定量。结果在10min内完成了氯酸盐和高氯酸盐的分离分析。氯酸盐和高氯酸盐在低中高3个添加水平的回收率为79.7%～96.4%,相对标准偏差小于5%(n=6),氯酸盐检出限为1.0μg/kg,高氯酸盐检出限为0.3μg/kg。结论该方法准确、可靠,可同时检测婴幼儿配方奶粉中氯酸盐和高氯酸盐的含量。
Objective To establish a method for determination of chlorate and perchlorate in infant formula milk powder by ion chromatography tandem mass spectrometry(IC-MS/MS). Methods The sample was extracted,purified to remove the protein and fat material, then separated by IC, and determined by electrospray ionization tandem mass spectrometry, with ~(18)O_3 chlorate and ~(18)O_4 perchlorate used as isotopic internal standard for quantitative analysis. Results The separation and analysis of chlorate and perchlorate were completed within 10 min. The recoveries were ranged from 79.7% to 96.4% for chlorate and perchlorate at 3 spiked levels. The relative standard deviations(RSDs) were less than 5%(n=6), and the limits of detection(LODs) for chlorate and perchlorate were 1.0μg/kg and 0.3 μg/kg, respectively. Conclusion This method is accurate and reliable, which is suitable for the determination of chlorate and perchlorate in infant formula milk powder.
Objective To establish a method for determination of chlorate and perchlorate in infant formula milk powder by ion chromatography tandem mass spectrometry(IC-MS/MS). Methods The sample was extracted,purified to remove the protein and fat material, then separated by IC, and determined by electrospray ionization tandem mass spectrometry, with ~(18)O_3 chlorate and ~(18)O_4 perchlorate used as isotopic internal standard for quantitative analysis. Results The separation and analysis of chlorate and perchlorate were completed within 10 min. The recoveries were ranged from 79.7% to 96.4% for chlorate and perchlorate at 3 spiked levels. The relative standard deviations(RSDs) were less than 5%(n=6), and the limits of detection(LODs) for chlorate and perchlorate were 1.0μg/kg and 0.3 μg/kg, respectively. Conclusion This method is accurate and reliable, which is suitable for the determination of chlorate and perchlorate in infant formula milk powder.
引文
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[19]张文龙.离子色谱法测定生活饮用水中溴酸盐和氯酸盐[J].化学工程师,2018,(5):33-35.Zhang WL.Determination of bromated and chlorate in drinking water by ion chromatography[J].Chem Eng,2018,(5):33-35.
[20]Pisarenko AN,Stanford BD,Qui?ones O,et al.Rapid analysis of perchlorate,chlorate and bromate ions in concentrated sodium hypochlorite solutions[J].Anal Chim Acta,2010,659(1):216-223.
[21]张景超.超高效液相色谱-串联质谱法测定茶叶中高氯酸盐[J].现代食品,2018,(9):144-146.Zhang JC.Determination of perchlorate in tea by ultra performance liquid chromatography-tandem mass spectrometry[J].Grain Distrib Technol,2018,(9):144-146.
[22]宋正规,张书芬,周子焱,等.超高效液相色谱-串联质谱同时测定茶叶中高氯酸盐和氯酸盐[J].茶叶科学,2017,37(6):597-604.Song ZG,Zhang SF,Zhou ZY,et al.Simultaneous determination of perchlorate and chlorate in tea by ultra-peryethylene liquid[J].J Tea Sci,2017,37(6):597-604.
[23]Aribi HE,Blanc YJCL,Antonsen S,et al.Analysis of perchlorate in foods and beverages by ion chromatography coupled with tandem mass spectrometry(IC-ESI-MS/MS)[J].Anal Chim Acta,2006,567(1):39-47.
[24]Valentín-Blasini L,Mauldin JP,Maple D,et al.Analysis of perchlorate in human urine using ion chromatography and electrospray tandem mass spectrometry[J].Anal Chem,2005,77(8):2475-2481.
[25]王浩,贾婧怡,张杉,等.液质联用法同时测定婴幼儿配方乳粉中氯酸盐和高氯酸盐残留[J].中国乳品工业,2019,47(2):48-50.Wang H,Jia JY,Zhang S,et al.Simultaneous determination of chlorate and perchlorate in infant milk powder by HPLC-MS/MS[J].Dairy Ind China,2019,47(2):48-50.
[26]Chen LY,Chen HS,Shen M,et al.Analysis of perchlorate in milk powder and milk by hydrophilic interaction chromatography combined with tandem mass spectrometry[J].J Agric Food Chem,2010,58(6):3736-3740.
[2]Murray CW.Environmental contaminants:Perchlorate[J].Encyclopedia Food Saf,2014,(2):337-341.
[3]蔡亚岐,史亚利,张萍,等.高氯酸盐的环境污染问题[J].化学进展,2006,18(11):1554-1564.Cai YQ,Shi YL,Zhang P,et al.Perchlorate related environmental problems[J].Prog Chem,2006,18(11):1554-1564.
[4]Yao L,Yang LX,Chen JM,et al.Levels,indoor-outdoor relationships and exposure risks of airborne particle-associated perchlorate and chlorate in two urban areas in Eastern Asia[J].Chemosphere,2015,(135):31-37.
[5]Shi YL,Zhang N,Gao JM,et al.Effect of fireworks display on perchlorate in air aerosols during the Spring Festival[J].Atmos Environ,2011,45(6):1323-1327.
[6]Kannan K,Praamsma ML,Oldi JF,et al.Occurrence of perchlorate in drinking water,groundwater,surface water and human saliva from India[J].Chemosphere,2009,76(1):22-26.
[7]闻自强,郑雯静,沈昊宇,等.高氯酸盐的危害、水污染现状与去除技术研究进展[J].环境化学,2019,38(1):209-216.Wen ZQ,Zheng WJ,Shen HY,et al.Research progress on the hazards,water pollution status and removal technique of perchlorate[J].Environ Chem,2019,38(1):209-216.
[8]Gan ZW,Sun HW,Wang RN,et al.Occurrence and exposure evaluation of perchlorate in outdoor dust and soil in mainland China[J].Sci Total Environ,2014,(470):99-106.
[9]Krynitsky AJ,Niemann RA,Nortrup DA.Determination of perchlorate anion in foods by ion chromatography-tandem mass spectrometry[J].Anal Chem,2004,76(18):5518-5522.
[10]Calderón R,Godoy F,Escudey M,et al.A review of perchlorate(ClO4-)occurrence in fruits and vegetables[J].Environ Monit Assess,2017,189(2):82.
[11]Hao D,Xiao KJ,Xian YP,et al.A novel approach for simultaneous analysis of perchlorate(ClO4-)and bromate(BrO3-)in fruits and vegetables using modified QuEChERS combined with ultrahigh performance liquid chromatography-tandem mass spectrometry[J].Food Chem,2019,(270):196-203.
[12]吴映璇,林峰,姚仰勋,等.固相萃取/(18)O标记高氯酸根稀释高效液相色谱-串联质谱法测定水果中的高氯酸盐[J].分析测试学报,2016,35(3):355-358.Wu YX,Lin F,Yao YX,et al.Determination of perchlorate in fruits by solid phase extraction/18O labeled perchlorate dilution high performance liquid chromatography-tandem mass spectrometry[J].J Instrum Anal,2016,35(3):355-358.
[13]宇盛好,李亦奇,张旭晟,等.上海市市售食品中高氯酸盐污染的暴露评估[J].上海预防医学,2017,29(6):426-430.Yu SH,Li YQ,Zhang XS,et al.Perchlorate contamination exposure assessment on commercial foods in Shanghai[J].Shanghai J Prev Med,2017,29(6):426-430.
[14]Kirk AB,Smith EE,Tian K,et al.Perchlorate in milk[J].Environ Sci Technol,2003,37(21):4979-4981.
[15]毕瑞锋.高效液相色谱-串联质谱法测定牛奶中的高氯酸盐和氯酸盐[J].中国乳品工业,2018,46(2):49-51.Bi RF.Simultaneous determination of perchlorate and chlorate in milk by porous graphitic carbon column-high performance liquid chromatography-tandem mass spectrometry[J].Dairy Ind,2018,46(2):49-51.
[16]Carr JA,Muralis,Hu F,et al.Changes in gastric sodium-iodide symporter(NIS)activity are associated with differences in thyroid gland sensitivity to perchlorate during metamorphosis[J].Gen Comp Endocr,2015,(219):16-23.
[17]吴春笃,李顺,许小红,等.高氯酸盐的环境毒理学效应及其机制的研究进展[J].环境与健康杂志,2013,30(1):85-89.Wu CD,Li S,Xu XH,et al.Environmental toxicological effect and mechanism of perchlorate[J].J Environ Health,2013,30(1):85-89.
[18]Wagner HP,Pepich BV,Pohl C,et al.Selective method for the analysis of perchlorate in drinking waters at nanogram per liter levels,using two-dimensional ion chromatography with suppressed conductivity detection[J].J Chromatogr A,2007,1155(1):15-21.
[19]张文龙.离子色谱法测定生活饮用水中溴酸盐和氯酸盐[J].化学工程师,2018,(5):33-35.Zhang WL.Determination of bromated and chlorate in drinking water by ion chromatography[J].Chem Eng,2018,(5):33-35.
[20]Pisarenko AN,Stanford BD,Qui?ones O,et al.Rapid analysis of perchlorate,chlorate and bromate ions in concentrated sodium hypochlorite solutions[J].Anal Chim Acta,2010,659(1):216-223.
[21]张景超.超高效液相色谱-串联质谱法测定茶叶中高氯酸盐[J].现代食品,2018,(9):144-146.Zhang JC.Determination of perchlorate in tea by ultra performance liquid chromatography-tandem mass spectrometry[J].Grain Distrib Technol,2018,(9):144-146.
[22]宋正规,张书芬,周子焱,等.超高效液相色谱-串联质谱同时测定茶叶中高氯酸盐和氯酸盐[J].茶叶科学,2017,37(6):597-604.Song ZG,Zhang SF,Zhou ZY,et al.Simultaneous determination of perchlorate and chlorate in tea by ultra-peryethylene liquid[J].J Tea Sci,2017,37(6):597-604.
[23]Aribi HE,Blanc YJCL,Antonsen S,et al.Analysis of perchlorate in foods and beverages by ion chromatography coupled with tandem mass spectrometry(IC-ESI-MS/MS)[J].Anal Chim Acta,2006,567(1):39-47.
[24]Valentín-Blasini L,Mauldin JP,Maple D,et al.Analysis of perchlorate in human urine using ion chromatography and electrospray tandem mass spectrometry[J].Anal Chem,2005,77(8):2475-2481.
[25]王浩,贾婧怡,张杉,等.液质联用法同时测定婴幼儿配方乳粉中氯酸盐和高氯酸盐残留[J].中国乳品工业,2019,47(2):48-50.Wang H,Jia JY,Zhang S,et al.Simultaneous determination of chlorate and perchlorate in infant milk powder by HPLC-MS/MS[J].Dairy Ind China,2019,47(2):48-50.
[26]Chen LY,Chen HS,Shen M,et al.Analysis of perchlorate in milk powder and milk by hydrophilic interaction chromatography combined with tandem mass spectrometry[J].J Agric Food Chem,2010,58(6):3736-3740.