加压毛细管电色谱法分离检测薯片中丙烯酰胺的含量
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摘要
建立加压毛细管电色谱法检测薯片中丙烯酰胺含量的方法。该方法采用EP-100-20/45-3-C18毛细管色谱柱(总长度45 cm,有效长度20 cm,直径100μm,ODS填料3μm)进行分离,并对流动相中有机相比例、磷酸盐缓冲溶液浓度、分离电压等实验条件进行考察和优化。结果表明:在流动相为乙腈-15 mmol/L NaH2PO4(pH 4.7)缓冲盐溶液(15∶85,V/V),流动相流速为0.04 mL/min,分离电压为-2 kV,紫外检测波长为202 nm的条件下,薯片中的丙烯酰胺得到了良好地分离。方法在2.0～32μg/mL范围内线性关系良好,相关系数为0.999 4。丙烯酰胺检出限(RSN=3)为0.30μg/mL,平均回收率为95.3%～108.1%,相对标准偏差低于1.48%。该方法已经用于薯片中丙烯酰胺含量测定,结果良好。
An efficient pressurized capillary electrochromatography(pCEC) method was developed for the determination of acrylamide in potato chips. The separation was performed on a reversed-phase EP-100-20/45-3-C18 capillary column(total length 45 cm, effective length 20 cm, diameter 100 μm, ODS packing 3 μm). Moreover, the mobile phase composition, the concentration of phosphate buffer, separation voltage and other experimental conditions were investigated and optimized, respectively. The mobile phase was composed of a mixture of acetonitrile and 15 mmol/L NaH2 PO4(pH 4.7)(15:85, V/V) at a flow rate of 0.04 mL/min. Under the optimal conditions(separation voltage-2 kV, and UV detection wavelength 202 nm), the analyte was well separated. The linear range was 2.0–32 μg/m L with a correlation coefficient of 0.999 4. The detection limit(LOD) of acrylamide was 0.30 μg/m L(RSN = 3). The average recoveries were 95.3%–108.1%, with a relative standard deviation(RSD) less than 1.48%. The method has been used for the determination of acrylamide in potato chips with good results.
An efficient pressurized capillary electrochromatography(pCEC) method was developed for the determination of acrylamide in potato chips. The separation was performed on a reversed-phase EP-100-20/45-3-C18 capillary column(total length 45 cm, effective length 20 cm, diameter 100 μm, ODS packing 3 μm). Moreover, the mobile phase composition, the concentration of phosphate buffer, separation voltage and other experimental conditions were investigated and optimized, respectively. The mobile phase was composed of a mixture of acetonitrile and 15 mmol/L NaH2 PO4(pH 4.7)(15:85, V/V) at a flow rate of 0.04 mL/min. Under the optimal conditions(separation voltage-2 kV, and UV detection wavelength 202 nm), the analyte was well separated. The linear range was 2.0–32 μg/m L with a correlation coefficient of 0.999 4. The detection limit(LOD) of acrylamide was 0.30 μg/m L(RSN = 3). The average recoveries were 95.3%–108.1%, with a relative standard deviation(RSD) less than 1.48%. The method has been used for the determination of acrylamide in potato chips with good results.
引文
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[14]玛尔江·巴哈提别克.应用加压毛细管电色谱技术检测鸡蛋中农兽药残留的研究[D].上海:上海交通大学,2011:7-9.
[15]山梅,李静,茹鑫,等.固相萃取-加压毛细管电色谱法测定水体中8种农药残留[J].分析科学学报,2015,31(4):445-449.DOI:10.13526/j.issn.1006-6144.2015.04.001.
[16]郭启雷,史海良,赵丽,等.加压毛细管电色谱测定乳及乳制品中三聚氰胺[J].食品研究与开发,2015,36(8):77-80.DOI:10.3969/j.issn.1005-6521.2015.08.021.
[17]万青云,茹鑫,王晓曦,等.加压毛细管电色谱-激光诱导荧光法检测4种黄曲霉毒素[J].分析化学,2015,43(7):1063-1068.DOI:10.11895/j.issn.0253-3820.150050.
[18]OUYANG X K,LUO Y Y,WEN Z S,et al.Simultaneous determination of flumequine and oxolinic acid residues in aquatic products using pressurized capillary electrochromatography[J].Food Analytical Methods,2014,7(9):1770-1775.DOI:10.1007/s12161-014-9818-6.
[19]王玉红,王彦,阎超.加压毛细管电色谱-微流蒸发光散射检测联用仪检测果糖、葡萄糖和蔗糖[J].广东化工,2017,44(16):63-66.DOI:10.3969/j.issn.1007-1865.2017.16.029.
[20]薛羚伟,胡代玉,张秋月,等.加压毛细管电色谱-固相萃取测定链格孢霉毒素[J].食品研究与开发,2017,38(8):100-104.DOI:10.3969/j.issn.1005-6521.2017.08.022.
[21]CHEN Z B,ZHANG L,LU Q M,et al.On-line concentration and pressurized capillary electrochromatography analysis of fiveagonists in human urine using a methacrylate monolithic column[J].Electrophoresis,2015,36(21/22):2720-2726.DOI:10.1002/elps.201500229.
[22]WU Y M,WANG X C,WU Q Z,et al.Separation and determination of structurally related free bile acids by pressurized capillary electrochromatography coupled to laser induced fluorescence detection[J].Analytical Methods,2010,2(12):1927-1933.DOI:10.1039/c0ay00309c.
[23]郑署,施文君,王晓曦,等.加压毛细管电色谱-紫外法检测复方维生素片中4种脂溶性维生素[J].食品科学,2014,35(20):105-109.DOI:10.7506/spkx1002-6630-201420021.
[24]YANG B,ZHANG X Y,ZHANG R S.A comparative study on analytical method of total alkaloids from cortex Phellodendri amurens by reversed phase high performance liquid chromatography(RP-HPLC)and pressurized capillary electrochromatography(pCEC)[J].Revista Brasileira de Farmacognosia-Brazilian Journal of Pharmacognosy,2011,21(1):16-23.DOI:10.1590/S0102-695X2011005000006.
[25]WU Y M,LIN J A,WU Q Z,et al.Rapid analysis of trace levels of flavins by pressurized capillary electrochromatography-laser induced fluorescence detection with sulfonated N-octadecyl methacrylate monolith[J].Journal of Pharmaceutical and Biomedical Analysis,2010,53(5):1324-1331.DOI:10.1016/j.jpba.2010.07.012.
[26]周文莉,阚文彬,王玉红,等.微流蒸发光散射检测器与加压毛细管电色谱联用测定川贝枇杷糖浆中6种有效成分的含量[J].分析测试学报,2015,34(3):321-327.DOI:10.3969/j.issn.1004-4957.2015.03.011.
[27]胡延,李利军,赵彦勇,等.加压毛细管电色谱分离检测升麻中阿魏酸与异阿魏酸[J].分析试验室,2015,34(3):347-350.DOI:10.13595/j.cnki.issn1000-0720.2015.0077.
[28]肖晓茹,冯军,程昊,等.加压毛细管电色谱分离检测虎杖根中蒽醌类成分[J].分析测试学报,2017,36(3):388-392.DOI:10.3969/j.issn.1004-4957.2017.03.016.
[29]高红秀,周文莉,王玉红,等.加压毛细管电色谱-微流蒸发光散射检测器联用系统的构建及其应用[J].分析化学,2014,42(5):766-772.DOI:10.3724/SP.J.1096.2014.31026.
[30]何秀丽,谭兴和,王燕,等.高效液相色谱法测定油炸马铃薯片中丙烯酰胺的含量[J].食品科学,2008,29(6):288-291.DOI:10.3321/j.issn:1002-6630.2008.06.061.
[2]SAHIN S,SUMNU G,OZTOP M H.Effect of osmotic pretreatment and microwave frying on acrylamide formation in potato strips[J].Journal of the Science of Food&Agriculture,2007,87(15):2830-2836.DOI:10.1002/jsfa.3034.
[3]曾稳稳,刘玉环,阮榕生,等.美拉德反应所引起的食品安全问题的研究进展[J].食品工业科技,2011,32(7):447-450.
[4]DEARFIELD K L,ABERNATHY C O,OTTLEY M S,et al.Acrylamide:its metabolism,developmental and reproductive effects,genotoxicity,and carcinogenicity[J].Mutation Research Fundamental&Molecular Mechanisms of Mutagenesis,1988,195(1):45-77.DOI:10.1016/0165-1110(88)90015-2.
[5]HU Q,XU X,LI Z,et al.Detection of acrylamide in potato chips using a fluorescent sensing method based on acrylamide polymerizationinduced distance increase between quantum dots[J].Biosensors Bioelectronics,2014,54(12):64-71.DOI:10.1016/j.bios.2013.10.046.
[6]束琴霞,石光辉,卢伟,等.扬州市油炸食品中丙烯酰胺的调查和分析[J].中国卫生检验杂志,2014,24(2):268-269.
[7]KALITA D,HOLM D G,JAYANTY S S.Role of polyphenols in acrylamide formation in the fried products of potato tubers with colored flesh[J].Food Research International,2013,54(1):753-759.DOI:10.1016/j.foodres.2013.08.023.
[8]KARASEK L,WENZL T,ANKLAM E.Determination of acrylamide in roasted chestnuts and chestnut-based foods by isotope dilution HPLC-MS/MS[J].Food Chemistry,2009,114(4):1555-1558.DOI:10.1016/j.foodchem.2008.11.057.
[9]ZHANG Y,REN Y,JIAO J,et al.Ultra high-performance liquid chromatography-tandem mass spectrometry for the simultaneous analysis of asparagine,sugars and acrylamide in Maillard reactions[J].Analytical Chemistry,2011,83(9):3297-3304.DOI:10.1021/ac1029538.
[10]蔡文,谭兴和,张喻,等.固相萃取-高效液相色谱法测定复合薯片中丙烯酰胺[J].激光生物学报,2014,23(2):178-182.DOI:10.3969/j.issn.1007-7146.2014.02.014.
[11]ZHAO H D,QIAO X G,DAI B Y,et al.Preparation and application of immobilised ionic liquid in solid-phase extraction for determination of trace acrylamide in food samples coupled with high-performance liquid chromatography[J].Journal of the Science of Food and Agriculture,2014,94(9):1787-1793.DOI:10.1002/jsfa.6493.
[12]殷斌,吴友谊,周震华,等.基质固相分散萃取-毛细管电泳测定米制品中丙烯酰胺[J].分析测试学报,2017,36(2):280-283.DOI:10.3969/j.issn.1004-4957.2017.02.023.
[13]ZHOU X,FAN L Y,ZHANG W,et al.Separation and determination of acrylamide in potato chips by micellar electrokinetic capillary chromatography[J].Talanta,2007,71(4):1541-1545.DOI:10.1016/j.talanta.2006.07.037.
[14]玛尔江·巴哈提别克.应用加压毛细管电色谱技术检测鸡蛋中农兽药残留的研究[D].上海:上海交通大学,2011:7-9.
[15]山梅,李静,茹鑫,等.固相萃取-加压毛细管电色谱法测定水体中8种农药残留[J].分析科学学报,2015,31(4):445-449.DOI:10.13526/j.issn.1006-6144.2015.04.001.
[16]郭启雷,史海良,赵丽,等.加压毛细管电色谱测定乳及乳制品中三聚氰胺[J].食品研究与开发,2015,36(8):77-80.DOI:10.3969/j.issn.1005-6521.2015.08.021.
[17]万青云,茹鑫,王晓曦,等.加压毛细管电色谱-激光诱导荧光法检测4种黄曲霉毒素[J].分析化学,2015,43(7):1063-1068.DOI:10.11895/j.issn.0253-3820.150050.
[18]OUYANG X K,LUO Y Y,WEN Z S,et al.Simultaneous determination of flumequine and oxolinic acid residues in aquatic products using pressurized capillary electrochromatography[J].Food Analytical Methods,2014,7(9):1770-1775.DOI:10.1007/s12161-014-9818-6.
[19]王玉红,王彦,阎超.加压毛细管电色谱-微流蒸发光散射检测联用仪检测果糖、葡萄糖和蔗糖[J].广东化工,2017,44(16):63-66.DOI:10.3969/j.issn.1007-1865.2017.16.029.
[20]薛羚伟,胡代玉,张秋月,等.加压毛细管电色谱-固相萃取测定链格孢霉毒素[J].食品研究与开发,2017,38(8):100-104.DOI:10.3969/j.issn.1005-6521.2017.08.022.
[21]CHEN Z B,ZHANG L,LU Q M,et al.On-line concentration and pressurized capillary electrochromatography analysis of fiveagonists in human urine using a methacrylate monolithic column[J].Electrophoresis,2015,36(21/22):2720-2726.DOI:10.1002/elps.201500229.
[22]WU Y M,WANG X C,WU Q Z,et al.Separation and determination of structurally related free bile acids by pressurized capillary electrochromatography coupled to laser induced fluorescence detection[J].Analytical Methods,2010,2(12):1927-1933.DOI:10.1039/c0ay00309c.
[23]郑署,施文君,王晓曦,等.加压毛细管电色谱-紫外法检测复方维生素片中4种脂溶性维生素[J].食品科学,2014,35(20):105-109.DOI:10.7506/spkx1002-6630-201420021.
[24]YANG B,ZHANG X Y,ZHANG R S.A comparative study on analytical method of total alkaloids from cortex Phellodendri amurens by reversed phase high performance liquid chromatography(RP-HPLC)and pressurized capillary electrochromatography(pCEC)[J].Revista Brasileira de Farmacognosia-Brazilian Journal of Pharmacognosy,2011,21(1):16-23.DOI:10.1590/S0102-695X2011005000006.
[25]WU Y M,LIN J A,WU Q Z,et al.Rapid analysis of trace levels of flavins by pressurized capillary electrochromatography-laser induced fluorescence detection with sulfonated N-octadecyl methacrylate monolith[J].Journal of Pharmaceutical and Biomedical Analysis,2010,53(5):1324-1331.DOI:10.1016/j.jpba.2010.07.012.
[26]周文莉,阚文彬,王玉红,等.微流蒸发光散射检测器与加压毛细管电色谱联用测定川贝枇杷糖浆中6种有效成分的含量[J].分析测试学报,2015,34(3):321-327.DOI:10.3969/j.issn.1004-4957.2015.03.011.
[27]胡延,李利军,赵彦勇,等.加压毛细管电色谱分离检测升麻中阿魏酸与异阿魏酸[J].分析试验室,2015,34(3):347-350.DOI:10.13595/j.cnki.issn1000-0720.2015.0077.
[28]肖晓茹,冯军,程昊,等.加压毛细管电色谱分离检测虎杖根中蒽醌类成分[J].分析测试学报,2017,36(3):388-392.DOI:10.3969/j.issn.1004-4957.2017.03.016.
[29]高红秀,周文莉,王玉红,等.加压毛细管电色谱-微流蒸发光散射检测器联用系统的构建及其应用[J].分析化学,2014,42(5):766-772.DOI:10.3724/SP.J.1096.2014.31026.
[30]何秀丽,谭兴和,王燕,等.高效液相色谱法测定油炸马铃薯片中丙烯酰胺的含量[J].食品科学,2008,29(6):288-291.DOI:10.3321/j.issn:1002-6630.2008.06.061.