基于表面增强拉曼光谱的鸭肉中己烯雌酚残留检测
|
摘要
采用表面增强拉曼光谱(SERS)法建立了一种快速检测鸭肉中己烯雌酚(DES)残留的方法。采用单因素分析法确定了合成金胶所需的柠檬酸三钠、纳米金胶、含DES的鸭肉提取液和硫酸镁溶液的最优加入量以及拉曼光谱的较佳采集时间。对鸭肉做简单的前处理后,建立鸭肉中的DES残留检测的定量分析模型。再以鸭肉提取液中DES浓度与819cm~(-1)处特征峰峰强建立标准曲线方程,可达到0.5mg/L的最低检测浓度。根据标准曲线方程得到其预测集的决定系数(R~2)为0.969 0,预测均方根误差(RMSEP)为0.728 1mg/L,平均回收率为83%～133%。试验结果表明,该方法可用于鸭肉中DES残留检测。
An approach based on surface-enhanced Raman spectroscopy(SERS)was developed to rapidly detect the diethylstilbestrol residues in duck meat in this study.Firstly,the single factor analysis method was adopted to determine the optimal amounts of sodium citrate,Au nanoparticles,duck meat extract containing diethylstilbestrol and magnesium sulfate solution,as well as the optimal measurement time.The quantitative analysis model for the detection of DES residues in duck meat was established after a simple pretreatment for duck meat was done.Thereafter,based on the basis of the above study,the linear equation with minimum detection concentration of 0.5 mg/L was established using diethylstilbestrol concentrations in duck meat extract and Raman intensities at 819 cm~(-1).Furthermore,the R~2 value for prediction set was 0.969 0,and the root mean square error for prediction(RMSEP)with average recovery of 83% ～133% was 0.728 1 mg/L.The experimental results indicated that the method adopted in the present study could be applied to detect DES residues in duck meat.
An approach based on surface-enhanced Raman spectroscopy(SERS)was developed to rapidly detect the diethylstilbestrol residues in duck meat in this study.Firstly,the single factor analysis method was adopted to determine the optimal amounts of sodium citrate,Au nanoparticles,duck meat extract containing diethylstilbestrol and magnesium sulfate solution,as well as the optimal measurement time.The quantitative analysis model for the detection of DES residues in duck meat was established after a simple pretreatment for duck meat was done.Thereafter,based on the basis of the above study,the linear equation with minimum detection concentration of 0.5 mg/L was established using diethylstilbestrol concentrations in duck meat extract and Raman intensities at 819 cm~(-1).Furthermore,the R~2 value for prediction set was 0.969 0,and the root mean square error for prediction(RMSEP)with average recovery of 83% ～133% was 0.728 1 mg/L.The experimental results indicated that the method adopted in the present study could be applied to detect DES residues in duck meat.
引文
[1]林维宣,董伟峰,陈溪,等.气相色谱-质谱法同时检测动物组织中多种激素类兽药的残留量[J].色谱,2009,27(3):294-298.
[2]吉薇.表面增强拉曼光谱测定氯霉素及其琥珀酸钠的研究[D].无锡:江南大学,2013:1-9.
[3]朱自莹,顾仁敖,陆天虹.拉曼光谱在化学中的应用[M].沈阳:东北大学出版社,1998:1-6.
[4]马海宽,张旭,钟石磊,等.基于静电富集-表面增强拉曼光谱联用技术的抗生素检测[J].中国激光,2018,45(2):306-313.
[5]马君,孔德地,韩晓红,等.应用银溶胶膜探测水中抗生素的表面增强拉曼光谱研究[J].光谱学与光谱分析,2013,33(10):2 688-2 693.
[6]修梓侨,梅雪峰,孙秀平.激素类药品的拉曼光谱研究[J].长春理工大学学报:自然科学版,2015(5):120-122.
[7]彭义杰,刘木华,赵进辉,等.应用表面增强拉曼光谱法检测鸭肉中萘夫西林残留的研究[J].光谱学与光谱分析,2017,37(12):3 736-3 742.
[8]郭红青,刘木华,袁海超,等.表面增强拉曼光谱技术快速检测鸭肉中的土霉素[J].食品安全质量检测学报,2017,8(1):169-176.
[9]PENG Yi-jie,LIU Mu-hua,CHEN Xiong-fei,et al.Surfaceenhanced Raman spectroscopy coupled with gold nanoparticles for rapid detection of amoxicillin residues in duck meat[J].Spectroscopy Letters,2017,50(10):579-584.
[10]罗晓燕,林玉娜,刘莉治,等.固相萃取高效液相色谱法同时测定禽畜组织中雌雄性激素残留的研究[J].中国卫生检验杂志,2005(4):387-389.
[11]李维红,熊琳,高雅琴,等.HPLC法同时测定牛羊肉中4种雌激素的残留量[J].黑龙江畜牧兽医,2014(11):207-209.
[12]李卫玲,叶阳,周有祥,等.柠檬酸三钠法制备胶体金的工艺条件优化[J].湖北农业科学,2010(10):2 529-2 532.
[13]高书燕,张树霞,杨恕霞,等.表面增强拉曼散射活性基底[J].化学通报,2007,70(12):908-914.
[14]张亚南.多吡啶铜配合物的合成及与DNA的相互作用研究[D].新乡:河南师范大学,2013:38-51.
[2]吉薇.表面增强拉曼光谱测定氯霉素及其琥珀酸钠的研究[D].无锡:江南大学,2013:1-9.
[3]朱自莹,顾仁敖,陆天虹.拉曼光谱在化学中的应用[M].沈阳:东北大学出版社,1998:1-6.
[4]马海宽,张旭,钟石磊,等.基于静电富集-表面增强拉曼光谱联用技术的抗生素检测[J].中国激光,2018,45(2):306-313.
[5]马君,孔德地,韩晓红,等.应用银溶胶膜探测水中抗生素的表面增强拉曼光谱研究[J].光谱学与光谱分析,2013,33(10):2 688-2 693.
[6]修梓侨,梅雪峰,孙秀平.激素类药品的拉曼光谱研究[J].长春理工大学学报:自然科学版,2015(5):120-122.
[7]彭义杰,刘木华,赵进辉,等.应用表面增强拉曼光谱法检测鸭肉中萘夫西林残留的研究[J].光谱学与光谱分析,2017,37(12):3 736-3 742.
[8]郭红青,刘木华,袁海超,等.表面增强拉曼光谱技术快速检测鸭肉中的土霉素[J].食品安全质量检测学报,2017,8(1):169-176.
[9]PENG Yi-jie,LIU Mu-hua,CHEN Xiong-fei,et al.Surfaceenhanced Raman spectroscopy coupled with gold nanoparticles for rapid detection of amoxicillin residues in duck meat[J].Spectroscopy Letters,2017,50(10):579-584.
[10]罗晓燕,林玉娜,刘莉治,等.固相萃取高效液相色谱法同时测定禽畜组织中雌雄性激素残留的研究[J].中国卫生检验杂志,2005(4):387-389.
[11]李维红,熊琳,高雅琴,等.HPLC法同时测定牛羊肉中4种雌激素的残留量[J].黑龙江畜牧兽医,2014(11):207-209.
[12]李卫玲,叶阳,周有祥,等.柠檬酸三钠法制备胶体金的工艺条件优化[J].湖北农业科学,2010(10):2 529-2 532.
[13]高书燕,张树霞,杨恕霞,等.表面增强拉曼散射活性基底[J].化学通报,2007,70(12):908-914.
[14]张亚南.多吡啶铜配合物的合成及与DNA的相互作用研究[D].新乡:河南师范大学,2013:38-51.