高效液相色谱法测定食品中脱氢乙酸的不确定度评定
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摘要
目的评定高效液相色谱法测定食品中脱氢乙酸测定的不确定度。方法依据JJF1059.1-2012《测量不确定度评定与表示》及新版国标方法 GB 5009.121-2016《食品安全国家标准食品中脱氢乙酸的测定》,建立评定脱氢乙酸不确定度的模型,对检测过程中各分量因素进行不确定度的分析评定。结果当样品中脱氢乙酸的含量为0.243 g/kg时,其扩展不确定度为0.070 g/kg, k=2。结论在整个实验过程中,标准品的配制及高效液相色谱仪的稳定性是影响实验结果的最主要因素,需严格把控。
Objective To evaluate the uncertainty for the determination of dehydroacetic acid in food by high performance liquid chromatography(HPLC). Methods According to JJF 1059.1-2012 Measurement uncertainty evaluation and expression and the new national standard method, GB 5009.121-2016 Detection of dehydroacetic acid in food, the model for assessing the uncertainty of dehydroacetic acid was established, to evaluate the uncertainty of component factors in dehydroacetic acid detection. Results When the content of dehydroacetic acid in the sample was 0.243 g/kg, the extended uncertainty was 0.070 g/kg, k=2. Conclusion During the whole test, the preparation of standard solution and the stability of HPLC are the key to the accurate detection of dehydroacetic acid in food which need to be strictly controlled
Objective To evaluate the uncertainty for the determination of dehydroacetic acid in food by high performance liquid chromatography(HPLC). Methods According to JJF 1059.1-2012 Measurement uncertainty evaluation and expression and the new national standard method, GB 5009.121-2016 Detection of dehydroacetic acid in food, the model for assessing the uncertainty of dehydroacetic acid was established, to evaluate the uncertainty of component factors in dehydroacetic acid detection. Results When the content of dehydroacetic acid in the sample was 0.243 g/kg, the extended uncertainty was 0.070 g/kg, k=2. Conclusion During the whole test, the preparation of standard solution and the stability of HPLC are the key to the accurate detection of dehydroacetic acid in food which need to be strictly controlled
引文
[1]曾金,王天地.食品中脱氢乙酸分析方法的最新研究进展[J].安徽农业科学,2016,44(15):82-83.Zeng J,Wang TD.Recent research progress on analytical methods of dehydroacetic in food[J].J Anhui Agric Sci,2016,44(15):82-83.
[2]张小芳,付大友.高效液相色谱法同时测定食醋和酱油中的6种防腐剂和甜味剂[J].中国调味品,2018,43(9):147-150.Zhang XF,Fu DY.Simultaneous determination of six preservatives and sweeteners in vinegar and soy sauce by HPLC[J].China Cond,2018,43(9):147-150.
[3]张倩勉,邓玉秀,刘星,等.HPLC法同时检测多种防腐剂的研究[J].食品科技,2018,(12):341-344,348.Zhang QM,Deng YX,Liu X,et al.The research of simultaneous determination of preservatives by HPLC[J].Food Sci Technol,2018,(12):341-344,348.
[4]周纯洁,牟兴川,朱永红,等.高效液相色谱法同时测定酱油中13种防腐剂[J].中国调味品,2016,(2):107-109,113.Zhou CJ,Mou XC,Zhu YH,et al.Simultaneous determination of 13preservatives in soy sauce by high performance liquid chromatography[J].China Cond,2016,(2):107-109,113.
[5]刘锐萍,朱娜,杨帛,等.高效液相色谱法同时测定食品中多种防腐剂含量方法的不确定度评定[J].饮料工业,2015,18(6):30-34.Liu RP,Zhu N,Yang B,et al.Evaluation of the uncertainty for the simultaneous determination of preservatives in foods using HPLC method[J].Bever Ind,2015,18(6):30-34.
[6]GB 2760-2014国家食品安全标准食品添加剂限量[S].GB 2760-2014 National food safety standard-Limit of additives in food[S].
[7]GB 5009.121-2016食品中脱氢乙酸的测定[S].GB 5009.121-2016 The detection of dehydroacetic acid in food[S].
[8]郝丽丽,任慧.浅谈检测实验室的测量不确定度评定[J].航空标准化与质量,2013,(4):49-52.Hao LL,Ren H.Discussion on the evaluation of uncertainty of testing laboratory[J].Aeronaut Stand Qual,2013,(4):49-52.
[9]徐渊金,林晓飞,陈含笑,等.高效液相色谱法测定酱油中山梨酸的不确定度评定[J].中国调味品,2015,(12):60-63,72.Xu YJ,Lin XF,Chen HX,et al.Uncertainty evaluation of sorbic acid in soy sauce detected by HPLC[J].China Condiment,2015,(12):60-63,72.
[10]李卓,陈冬,舒蕊华,等.高效液相色谱法测定辣椒粉中辣椒素的不确定度评定[J].中国调味品,2017,42(5):135-137,148.Li Z,Chen D,Shu RH,et al.Uncertainty evaluation for determination of capsaicin in cayenne pepper by HPLC[J].China Cond,2017,42(5):135-137,148.
[11]陈毓芳,林海丹,官咏仪,等.高效液相色谱法测定饮料中乙基麦芽酚含量的不确定度评定[J].食品安全质量检测学报,2018,9(9):2175-2180.Chen YF,Lin HD,Guan YY,et al.Uncertainty evaluation for determination of ethyl maltol in beverages by high performance liquid chromatography[J].J Food Saf Qual,2018,9(9):2175-2180.
[12]JJF 1059.1-2012测量不确定度评定与表示[S].JJF 1059.1-2012 Evaluation and expression of uncertainty in measurement[S].
[13]赵欣,李强.高效液相色谱法测定面包、饼干等烘焙类食品中的脱氢乙酸[J].食品安全质量检测学报,2018,9(13):3464-3468.Zhao X,Li Q.Quantitative determination of dehydroacetic acid in bread,cookies and other baked food by high performance liquid chromatography[J].J Food Saf Qual,2018,9(13):3464-3468.
[14]Lee MJ,Lee JM,Kim S,et al.Simultaneous analysis and measurement of uncertainty estimation of six isoflavones in Cheonggukjang by liquid chromatography-electrospray tandem mass spectrometry[J].Food Chem,2019,289(8):139-134.
[15]赵天珍.气相色谱法测定月饼中脱氢乙酸的不确定度评定[J].食品机械,2011,27(4):84-86.Zhao TZ.Uncertainty evaluation about the determination results of dehydroacetic acid in mooncakes by gas chromatography[J].Food Mach,2011,27(4):84-86.
[16]JJG 196-2006常用玻璃量器检定规程[S].JJG 196-2006 Verification method of the working glass container[S].
[2]张小芳,付大友.高效液相色谱法同时测定食醋和酱油中的6种防腐剂和甜味剂[J].中国调味品,2018,43(9):147-150.Zhang XF,Fu DY.Simultaneous determination of six preservatives and sweeteners in vinegar and soy sauce by HPLC[J].China Cond,2018,43(9):147-150.
[3]张倩勉,邓玉秀,刘星,等.HPLC法同时检测多种防腐剂的研究[J].食品科技,2018,(12):341-344,348.Zhang QM,Deng YX,Liu X,et al.The research of simultaneous determination of preservatives by HPLC[J].Food Sci Technol,2018,(12):341-344,348.
[4]周纯洁,牟兴川,朱永红,等.高效液相色谱法同时测定酱油中13种防腐剂[J].中国调味品,2016,(2):107-109,113.Zhou CJ,Mou XC,Zhu YH,et al.Simultaneous determination of 13preservatives in soy sauce by high performance liquid chromatography[J].China Cond,2016,(2):107-109,113.
[5]刘锐萍,朱娜,杨帛,等.高效液相色谱法同时测定食品中多种防腐剂含量方法的不确定度评定[J].饮料工业,2015,18(6):30-34.Liu RP,Zhu N,Yang B,et al.Evaluation of the uncertainty for the simultaneous determination of preservatives in foods using HPLC method[J].Bever Ind,2015,18(6):30-34.
[6]GB 2760-2014国家食品安全标准食品添加剂限量[S].GB 2760-2014 National food safety standard-Limit of additives in food[S].
[7]GB 5009.121-2016食品中脱氢乙酸的测定[S].GB 5009.121-2016 The detection of dehydroacetic acid in food[S].
[8]郝丽丽,任慧.浅谈检测实验室的测量不确定度评定[J].航空标准化与质量,2013,(4):49-52.Hao LL,Ren H.Discussion on the evaluation of uncertainty of testing laboratory[J].Aeronaut Stand Qual,2013,(4):49-52.
[9]徐渊金,林晓飞,陈含笑,等.高效液相色谱法测定酱油中山梨酸的不确定度评定[J].中国调味品,2015,(12):60-63,72.Xu YJ,Lin XF,Chen HX,et al.Uncertainty evaluation of sorbic acid in soy sauce detected by HPLC[J].China Condiment,2015,(12):60-63,72.
[10]李卓,陈冬,舒蕊华,等.高效液相色谱法测定辣椒粉中辣椒素的不确定度评定[J].中国调味品,2017,42(5):135-137,148.Li Z,Chen D,Shu RH,et al.Uncertainty evaluation for determination of capsaicin in cayenne pepper by HPLC[J].China Cond,2017,42(5):135-137,148.
[11]陈毓芳,林海丹,官咏仪,等.高效液相色谱法测定饮料中乙基麦芽酚含量的不确定度评定[J].食品安全质量检测学报,2018,9(9):2175-2180.Chen YF,Lin HD,Guan YY,et al.Uncertainty evaluation for determination of ethyl maltol in beverages by high performance liquid chromatography[J].J Food Saf Qual,2018,9(9):2175-2180.
[12]JJF 1059.1-2012测量不确定度评定与表示[S].JJF 1059.1-2012 Evaluation and expression of uncertainty in measurement[S].
[13]赵欣,李强.高效液相色谱法测定面包、饼干等烘焙类食品中的脱氢乙酸[J].食品安全质量检测学报,2018,9(13):3464-3468.Zhao X,Li Q.Quantitative determination of dehydroacetic acid in bread,cookies and other baked food by high performance liquid chromatography[J].J Food Saf Qual,2018,9(13):3464-3468.
[14]Lee MJ,Lee JM,Kim S,et al.Simultaneous analysis and measurement of uncertainty estimation of six isoflavones in Cheonggukjang by liquid chromatography-electrospray tandem mass spectrometry[J].Food Chem,2019,289(8):139-134.
[15]赵天珍.气相色谱法测定月饼中脱氢乙酸的不确定度评定[J].食品机械,2011,27(4):84-86.Zhao TZ.Uncertainty evaluation about the determination results of dehydroacetic acid in mooncakes by gas chromatography[J].Food Mach,2011,27(4):84-86.
[16]JJG 196-2006常用玻璃量器检定规程[S].JJG 196-2006 Verification method of the working glass container[S].