高效液相色谱法测定鳕鱼中孔雀石绿含量的不确定度评定
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摘要
目的评定高效液相色谱法测定鳕鱼中孔雀石绿(malachite green, MG)含量的不确定度。方法通过建立数学模型,对高效液相色谱法(high performance liquid chromatography, HPLC)测定鳕鱼中孔雀石绿含量进行不确定度评定,分析不确定来源及其对测定过程中不确定度的相对贡献,并计算合成不确定度,最终得到鳕鱼中孔雀石绿的扩展不确定度。结果当鳕鱼中孔雀石绿含量为1.8822μg/kg时,在95%的置信区间下,合成不确定度为0.09644μg/kg,扩展不确定度为0.19288μg/kg (k=2)。结论实验过程的不确定度主要来源于标准曲线拟合,仪器重复测量和标准溶液配制以及试样称量、定容体积。本研究可为以后的检测工作提供可行性建议。
Objective To evaluate the uncertainty of determination of malachite green(MG) content in Gadus by high performance liquid chromatography(HPLC). Methods By establishing a mathematical model, the uncertainty of the determination of MG content in Gadus by HPLC was evaluated. The source of uncertainty and its relative contribution to the uncertainty in the determination process were analyzed, and the synthetic uncertainty was calculated. Finally, the extension uncertainty of malachite green in Gadus was obtained. Results When the MG content was 1.8822 μg/kg, the synthetic uncertainty was 0.09644 μg/kg and the extended uncertainty was 0.19288 μg/kg(k=2) under the 95% confidence interval. Conclusion The evaluation results show that the uncertainties of the experiment are mainly derived from curve fitting, measurement repeatability, standard solution preparation, weight and constant volume of sample. The article provides the feasible suggestions for the future inspection work.
Objective To evaluate the uncertainty of determination of malachite green(MG) content in Gadus by high performance liquid chromatography(HPLC). Methods By establishing a mathematical model, the uncertainty of the determination of MG content in Gadus by HPLC was evaluated. The source of uncertainty and its relative contribution to the uncertainty in the determination process were analyzed, and the synthetic uncertainty was calculated. Finally, the extension uncertainty of malachite green in Gadus was obtained. Results When the MG content was 1.8822 μg/kg, the synthetic uncertainty was 0.09644 μg/kg and the extended uncertainty was 0.19288 μg/kg(k=2) under the 95% confidence interval. Conclusion The evaluation results show that the uncertainties of the experiment are mainly derived from curve fitting, measurement repeatability, standard solution preparation, weight and constant volume of sample. The article provides the feasible suggestions for the future inspection work.
引文
[1]王群,宋怿,马兵.水产品中孔雀石绿的风险评估(一)[J].中国渔业质量与标准,2011,1(2):38-43.Wang Q,Song Y,Ma B.Risk assessment of malachite green in aquatic products[J].Chin Fishery Qual Standard,2011,1(2):38-43.
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[3]刘明扬,肖珊珊,于兵,等.水产品中孔雀石绿和结晶紫残留检测技术研究进展[J].食品安全质量检测学报,2015,6(1):35-40.Liu MY,Xiao SS,Yu B,et al.Research progress of the residue determination of triphenymethanedyes in aquatic product[J].J Food Saf Qual,2015,6(1):35-40.
[4]李凯华,张玲,闫清华,等.优化高效液相色谱-串联质谱法检测水产品中孔雀石绿及隐色孔雀石绿的残留量[J].食品安全质量检测学报,2018,9(6):1351-1357.Li KH,Zhang L,Yan QH,et al.Optimization of methods for determination of malachite green and leucomalachite green in aquatic products by high performance liquid chromatography-tandem mass spectrometry[J].J Food Saf Qual,2018,9(6):1351-1357.
[5]Fallah AA,Barani A.Determination of malachite green residues in farmed rainbow trout in Iran[J].Food Control,2014,40(1):100-105.
[6]向仲朝,岳蕴瑶,张婷,等.水产品中孔雀石绿和结晶紫及其代谢产物的高效液相色谱测定法[J].中国卫生检验杂志,2014,24(6):788-790.Xiang ZC,Yue YY,Zhang T,et al.Determination of the malachite green and crystal violet in aquatic products by HPLC[J].Chin J Health Lab Technol,2014,24(6):788-790.
[7]Turnipseed SB,Roybal JE,Hurlbut JA,et al.Gas chromatographic/MSspectrometric confirmation of leucomalachite green in catfish tissue[J].JAOAC Int,1995,78(4):971-977.
[8]梁高道,麦琦.气相色谱质谱法确认水产品中的孔雀石绿[J].公共卫生与预防医学,2009,20(6):69-71.Liang GD,Mai Q.Determination of malachite green in aquatic products by gas chromatography[J].J Pub Health and Prev Med,2009,20(6):69-71.
[9]陈湘艺,万译文,黄向荣,等.高效液相色谱-串联质谱法同时测定水产品中孔雀石绿及隐色孔雀石绿药物残留[J].中国卫生检验杂志,2013,23(12):2562-2565.Chen XY,Wan YW,Huang XR,et al.Simultaneous determination of malachite green and lecuomalachite green residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry[J].Chin J Health Lab Technol,2013,23(12):2562-2565.
[10]Stachowiak MO,Connolly LM,Stevenson P,et al.Development and validation of a fast monoclonal based disequilibrium enzyme-linked immunosorbent assay for the detection of triphenylmethane dyes and their metabolites in fish[J].Anal Chim Acta,2011,698(1-2):51-60.
[11]余孔捷,黄杰,刘正才,等.液质联用法测定水产品中孔雀石绿、结晶紫的不确定度评定[J].分析试验室,2008,27(S1):203-209.Yu KJ,Huang J,Liu ZC,et al.Uncertainty evaluation in determination of malachite green,crystal violet in aquatic products by liquid chromatography/mass spectrometry[J].Chin J Anal Lab,2008,27(S1):203-209.
[12]郑振光.液质联用法测定水产品中孔雀石绿的不确定度评定[J].福建质量信息,2008,(6):84-87.Zheng ZG.Uncertainty evaluation in determination of malachite green in aquatic products by liquid chromatography/mass spectrometry[J].Fujian Qual Inf,2008,(6):84-87.
[13]邵秋荣,方邢有,张群玲,等.水产品中孔雀石绿残留量的不确定度评定[J].中国农学通报,2007,23(4):105-107.Shao QR,Fang XY,Zhang QL,et al.The assessment of uncertainty of the malachite green residues in aquatic product[J].Chin Agric Sci Bull,2007,23(4):105-107.
[14]林敏,沈雨锋,潘圆圆,等.HPLC法测定水产品中孔雀石绿残留量的不确定度评定[J].中国卫生检验杂志,2010,20(8):2088-2090.Lin M,Shen YF,Pan YY,et al.Evaluation of uncertainty for detection of malachite green residue in aquatic product by HPLC[J].Chin J Health Lab Technol,2010,20(8):2088-2090.
[15]JJF 1135-2005化学分析测量不确定度评定[S].JJF 1135-2005 Evaluation of uncertainty in chemical analysis measurement[S].
[16]GB/T 20361-2006水产品中孔雀石绿和结晶紫残留量的测定高效液相色谱荧光检测法[S].GB/T 20361-2006 Determination of malachite green and gentian violet residues in fishery products-High performance liquid chromatography with fluorescence detector[S].
[17]JJG 1036-2008电子天平[S].JJG 1036-2008 Electronic balance[S].
[18]JJG 196-2006常用玻璃量器检定规程[S].JJG 196-2006 Verification regulation of working glass container[S].
[19]JJG 646-2006移液器检定规程[S].JJG 646-2006 Verification regulation of locomotive pipette[S].
[20]JJG 12-1987刻度离心管、刻度试管、血糖管、消化管检定规程[S].JJG12-1987 Verification regulation of graduated cantrifuge tubes,graduated test tubes blood sugar tubes and blood digestion tubes[S].
[2]徐向荣,郝青,彭加喜,等.水产品中残留孔雀石绿研究进展[J].热带海洋学报,2013,4(32):97-106.Xu XR,Hao Q,Peng JX,et al.Recent studies on residual malachite green in aquatic products[J].J Trop Oceanogr,2013,4(32):97-106.
[3]刘明扬,肖珊珊,于兵,等.水产品中孔雀石绿和结晶紫残留检测技术研究进展[J].食品安全质量检测学报,2015,6(1):35-40.Liu MY,Xiao SS,Yu B,et al.Research progress of the residue determination of triphenymethanedyes in aquatic product[J].J Food Saf Qual,2015,6(1):35-40.
[4]李凯华,张玲,闫清华,等.优化高效液相色谱-串联质谱法检测水产品中孔雀石绿及隐色孔雀石绿的残留量[J].食品安全质量检测学报,2018,9(6):1351-1357.Li KH,Zhang L,Yan QH,et al.Optimization of methods for determination of malachite green and leucomalachite green in aquatic products by high performance liquid chromatography-tandem mass spectrometry[J].J Food Saf Qual,2018,9(6):1351-1357.
[5]Fallah AA,Barani A.Determination of malachite green residues in farmed rainbow trout in Iran[J].Food Control,2014,40(1):100-105.
[6]向仲朝,岳蕴瑶,张婷,等.水产品中孔雀石绿和结晶紫及其代谢产物的高效液相色谱测定法[J].中国卫生检验杂志,2014,24(6):788-790.Xiang ZC,Yue YY,Zhang T,et al.Determination of the malachite green and crystal violet in aquatic products by HPLC[J].Chin J Health Lab Technol,2014,24(6):788-790.
[7]Turnipseed SB,Roybal JE,Hurlbut JA,et al.Gas chromatographic/MSspectrometric confirmation of leucomalachite green in catfish tissue[J].JAOAC Int,1995,78(4):971-977.
[8]梁高道,麦琦.气相色谱质谱法确认水产品中的孔雀石绿[J].公共卫生与预防医学,2009,20(6):69-71.Liang GD,Mai Q.Determination of malachite green in aquatic products by gas chromatography[J].J Pub Health and Prev Med,2009,20(6):69-71.
[9]陈湘艺,万译文,黄向荣,等.高效液相色谱-串联质谱法同时测定水产品中孔雀石绿及隐色孔雀石绿药物残留[J].中国卫生检验杂志,2013,23(12):2562-2565.Chen XY,Wan YW,Huang XR,et al.Simultaneous determination of malachite green and lecuomalachite green residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry[J].Chin J Health Lab Technol,2013,23(12):2562-2565.
[10]Stachowiak MO,Connolly LM,Stevenson P,et al.Development and validation of a fast monoclonal based disequilibrium enzyme-linked immunosorbent assay for the detection of triphenylmethane dyes and their metabolites in fish[J].Anal Chim Acta,2011,698(1-2):51-60.
[11]余孔捷,黄杰,刘正才,等.液质联用法测定水产品中孔雀石绿、结晶紫的不确定度评定[J].分析试验室,2008,27(S1):203-209.Yu KJ,Huang J,Liu ZC,et al.Uncertainty evaluation in determination of malachite green,crystal violet in aquatic products by liquid chromatography/mass spectrometry[J].Chin J Anal Lab,2008,27(S1):203-209.
[12]郑振光.液质联用法测定水产品中孔雀石绿的不确定度评定[J].福建质量信息,2008,(6):84-87.Zheng ZG.Uncertainty evaluation in determination of malachite green in aquatic products by liquid chromatography/mass spectrometry[J].Fujian Qual Inf,2008,(6):84-87.
[13]邵秋荣,方邢有,张群玲,等.水产品中孔雀石绿残留量的不确定度评定[J].中国农学通报,2007,23(4):105-107.Shao QR,Fang XY,Zhang QL,et al.The assessment of uncertainty of the malachite green residues in aquatic product[J].Chin Agric Sci Bull,2007,23(4):105-107.
[14]林敏,沈雨锋,潘圆圆,等.HPLC法测定水产品中孔雀石绿残留量的不确定度评定[J].中国卫生检验杂志,2010,20(8):2088-2090.Lin M,Shen YF,Pan YY,et al.Evaluation of uncertainty for detection of malachite green residue in aquatic product by HPLC[J].Chin J Health Lab Technol,2010,20(8):2088-2090.
[15]JJF 1135-2005化学分析测量不确定度评定[S].JJF 1135-2005 Evaluation of uncertainty in chemical analysis measurement[S].
[16]GB/T 20361-2006水产品中孔雀石绿和结晶紫残留量的测定高效液相色谱荧光检测法[S].GB/T 20361-2006 Determination of malachite green and gentian violet residues in fishery products-High performance liquid chromatography with fluorescence detector[S].
[17]JJG 1036-2008电子天平[S].JJG 1036-2008 Electronic balance[S].
[18]JJG 196-2006常用玻璃量器检定规程[S].JJG 196-2006 Verification regulation of working glass container[S].
[19]JJG 646-2006移液器检定规程[S].JJG 646-2006 Verification regulation of locomotive pipette[S].
[20]JJG 12-1987刻度离心管、刻度试管、血糖管、消化管检定规程[S].JJG12-1987 Verification regulation of graduated cantrifuge tubes,graduated test tubes blood sugar tubes and blood digestion tubes[S].