高效液相色谱法测定粮食中赭曲霉毒素A含量的不确定度评定
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摘要
对高效液相色谱法测定粮食中赭曲霉毒素A含量的测量不确定度进行评定。建立数学模型,分析不确定度来源,计算不确定度分量,并合成测量结果的不确定度。本次评定结果表明:赭曲霉毒素A测量结果的不确定度主要来自样品不均匀性、浓度、体积、称量、提取效率,重复性6个因素,其中浓度因素引入的不确定度分量贡献最大,其次是体积因素,而由试样称量因素引入的不确定度分量最小。高效液相色谱法测定粮食中赭曲霉毒素A的含量为4.48μg/kg时,其扩展不确定度为0.41μg/kg,k=2。
The measurement uncertainty of ochratoxin A in grain determined by high performance liquid chromatography was evaluated.A mathematical model was established,the sources of uncertainty were analyzed,the components of uncertainty were calculated,and the uncertainty of measurement results was synthesized.The results show that,the uncertainty of ochratoxin A content mainly comes from6 factors:sample heterogeneity,concentration,volume,sample weighing,extraction efficiency and repeatability.Among them,the uncertainty component contributed by the concentration factor is the most important,followed by the volume factor,and the uncertainty component introduced by the weighing factor is the smallest.When the ochratoxin A content is 4.48μg/kg in grain determined by high performance liquid chromatography,the expanded uncertainty is 0.41μg/kg,k=2.
The measurement uncertainty of ochratoxin A in grain determined by high performance liquid chromatography was evaluated.A mathematical model was established,the sources of uncertainty were analyzed,the components of uncertainty were calculated,and the uncertainty of measurement results was synthesized.The results show that,the uncertainty of ochratoxin A content mainly comes from6 factors:sample heterogeneity,concentration,volume,sample weighing,extraction efficiency and repeatability.Among them,the uncertainty component contributed by the concentration factor is the most important,followed by the volume factor,and the uncertainty component introduced by the weighing factor is the smallest.When the ochratoxin A content is 4.48μg/kg in grain determined by high performance liquid chromatography,the expanded uncertainty is 0.41μg/kg,k=2.
引文
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[2]Lalini R,Kanti B.Ochratoxins-Food Contaminants:Impact on Human Health[J].Toxins,2010,2(4):771-776.
[3]杜政,唐瑞明.粮食中真菌毒素标准、法规与检验[M].长沙:湖南科学技术出版社,2013:5-6.
[4]Pfohl-Leszkowicz A,Manderville R.Ochratoxin A:An overview on toxicity and carcinogenicity in animals and humans[J].Mol Nutr Food Res,2007,51(1):61-99.
[5]Grosso F,Sai6d S,Mabrouk I,et al.New data on the occurrence of ochratoxin A in human sera from patients affected or not by renal diseases in Tunisia[J].Food and Chemical Toxicology,2003,41(8):1133-1140.
[6]夏骏,李勇,徐国茂,等.动物源性食品中赭曲霉毒素A毒性和检测方法研究进展[J].江西畜牧兽医杂志,2015(2):4-7.
[7]Benford D,Boyle C,Dekant W,et al.Ochratoxin A Safety Evaluation of Certain Mycotoxins in Food[G].WHO Food Additives Series 47.FAO Food and Nutrition Paper,Switzerland,WHO Geneva,2001,74:281-415.
[8]GB2761—2017,食品安全国家标准食品中真菌毒素限量[S].
[9]GB5009.96—2016,食品安全国家标准食品中赭曲霉毒素A的测定[S].
[10]邵亮亮,赵美凤,宁晖,等.高效液相色谱法测定小麦中脱氧雪腐镰刀菌烯醇含量的不确定度评定[J].食品科学,2016,37(12):232-237.
[11]陆美斌,李为喜,武力,等.HPLC测定谷物中玉米赤霉烯酮的不确定度评定[J].中国粮油学报,2011,26(3):114-118.
[12]马振栋,王凤池,郝冬生.高效液相色谱柱后衍生法测定黄曲霉毒素的不确定度评定[J].计量学报,2002,3(3):229-232.
[13]曹阳,张艳,刘美辰.高效液相色谱法测定粮食中T-2毒素含量的不确定度评定[J].粮油食品科技,2013,21(06):70-72.
[14]Carina E M,Andrea L A,Stella M C,et al.Occurrence of ochratoxin A and ochratoxigenic mycoflora in corn and corn based foods and feeds in some South American countries[J].Mycopathologia,2007,163(5):249-260.
[15]Ahmad A,Jae-Hyuk Y.Occurrence,Toxicity,and Analysis of Major Mycotoxins in Food[J].International Journal of Environmental Research and Public Health,2017,14(12):632-645.
[16]梁桂娟,张琼,杨波.高效液相色谱-荧光检测法检测大米中的赭曲霉毒素A[J].中国酿造,2015,34(8):136-138.
[17]Wei M,Zhang W.The determination of Ochratoxin A based on the electrochemical aptasensor by carbon aerogels and methylene blue assisted signal amplification[J].Chem Cent J,2018,12(1):45-53.
[18]李万鹏,弓丽华,付爽.HPLC法测定粮谷中赭曲霉毒素A含量结果的不确定度评定[J].郑州轻工业学院学报:自然科学版,2015,30(Z1):20-25.
[19]宋卫得,高尧华,厉雪芹,等.高效液相色谱法测定饲料中赭曲霉毒素A的不确定度评估[J].粮食与饲料工业,2016,1(03):64-67.
[20]CNAS-GL006,化学分析中不确定度的评估指南[S].
[21]JJF1135—2005,化学分析测量不确定度评定[S].
[22]彭春红,王丽,安凤平,等.制粉和分层研磨对小麦中赭曲霉毒素A的去除效果[J].中国粮油学报,2016,31(3):7-11.
[23]王松雪,张喆.样品扦样与制备-真菌毒素准确分析中的决定性因素[J].检验检疫学,2010(5):61-62.
[24]JJF1059.1—2012,测量不确定度评定与表示[S].
[25]JJG196—2006,常用玻璃量器检定规程[S].
[26]JJG646—2006,移液器检定规程[S].
[27]周志红,赵乐宽.显著性检验及不确定度在实验室的应用[J].沈阳师范学院学报,2002,4(20):278-279.
[28]刘庆,万力,王新平,等.如何评估回收率测量结果不确定度[J].中国测试,2015,41(S1):82-84.
[29]宗亚娟,袁剑韬,刘国军.测量不确定度评定中应注意的一些问题[J].宇航计测技术,2011,31(02):60-62.
[2]Lalini R,Kanti B.Ochratoxins-Food Contaminants:Impact on Human Health[J].Toxins,2010,2(4):771-776.
[3]杜政,唐瑞明.粮食中真菌毒素标准、法规与检验[M].长沙:湖南科学技术出版社,2013:5-6.
[4]Pfohl-Leszkowicz A,Manderville R.Ochratoxin A:An overview on toxicity and carcinogenicity in animals and humans[J].Mol Nutr Food Res,2007,51(1):61-99.
[5]Grosso F,Sai6d S,Mabrouk I,et al.New data on the occurrence of ochratoxin A in human sera from patients affected or not by renal diseases in Tunisia[J].Food and Chemical Toxicology,2003,41(8):1133-1140.
[6]夏骏,李勇,徐国茂,等.动物源性食品中赭曲霉毒素A毒性和检测方法研究进展[J].江西畜牧兽医杂志,2015(2):4-7.
[7]Benford D,Boyle C,Dekant W,et al.Ochratoxin A Safety Evaluation of Certain Mycotoxins in Food[G].WHO Food Additives Series 47.FAO Food and Nutrition Paper,Switzerland,WHO Geneva,2001,74:281-415.
[8]GB2761—2017,食品安全国家标准食品中真菌毒素限量[S].
[9]GB5009.96—2016,食品安全国家标准食品中赭曲霉毒素A的测定[S].
[10]邵亮亮,赵美凤,宁晖,等.高效液相色谱法测定小麦中脱氧雪腐镰刀菌烯醇含量的不确定度评定[J].食品科学,2016,37(12):232-237.
[11]陆美斌,李为喜,武力,等.HPLC测定谷物中玉米赤霉烯酮的不确定度评定[J].中国粮油学报,2011,26(3):114-118.
[12]马振栋,王凤池,郝冬生.高效液相色谱柱后衍生法测定黄曲霉毒素的不确定度评定[J].计量学报,2002,3(3):229-232.
[13]曹阳,张艳,刘美辰.高效液相色谱法测定粮食中T-2毒素含量的不确定度评定[J].粮油食品科技,2013,21(06):70-72.
[14]Carina E M,Andrea L A,Stella M C,et al.Occurrence of ochratoxin A and ochratoxigenic mycoflora in corn and corn based foods and feeds in some South American countries[J].Mycopathologia,2007,163(5):249-260.
[15]Ahmad A,Jae-Hyuk Y.Occurrence,Toxicity,and Analysis of Major Mycotoxins in Food[J].International Journal of Environmental Research and Public Health,2017,14(12):632-645.
[16]梁桂娟,张琼,杨波.高效液相色谱-荧光检测法检测大米中的赭曲霉毒素A[J].中国酿造,2015,34(8):136-138.
[17]Wei M,Zhang W.The determination of Ochratoxin A based on the electrochemical aptasensor by carbon aerogels and methylene blue assisted signal amplification[J].Chem Cent J,2018,12(1):45-53.
[18]李万鹏,弓丽华,付爽.HPLC法测定粮谷中赭曲霉毒素A含量结果的不确定度评定[J].郑州轻工业学院学报:自然科学版,2015,30(Z1):20-25.
[19]宋卫得,高尧华,厉雪芹,等.高效液相色谱法测定饲料中赭曲霉毒素A的不确定度评估[J].粮食与饲料工业,2016,1(03):64-67.
[20]CNAS-GL006,化学分析中不确定度的评估指南[S].
[21]JJF1135—2005,化学分析测量不确定度评定[S].
[22]彭春红,王丽,安凤平,等.制粉和分层研磨对小麦中赭曲霉毒素A的去除效果[J].中国粮油学报,2016,31(3):7-11.
[23]王松雪,张喆.样品扦样与制备-真菌毒素准确分析中的决定性因素[J].检验检疫学,2010(5):61-62.
[24]JJF1059.1—2012,测量不确定度评定与表示[S].
[25]JJG196—2006,常用玻璃量器检定规程[S].
[26]JJG646—2006,移液器检定规程[S].
[27]周志红,赵乐宽.显著性检验及不确定度在实验室的应用[J].沈阳师范学院学报,2002,4(20):278-279.
[28]刘庆,万力,王新平,等.如何评估回收率测量结果不确定度[J].中国测试,2015,41(S1):82-84.
[29]宗亚娟,袁剑韬,刘国军.测量不确定度评定中应注意的一些问题[J].宇航计测技术,2011,31(02):60-62.
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