基于低场核磁共振(LF-NMR)弛豫特性的油脂品质检测研究
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摘要
研究了低场核磁共振(LF-NMR)检测过程中的仪器参数、检测温度及体积等对大豆油、棕榈油和猪油弛豫特性检测结果的影响,并给出了适用于含固态脂类油脂样品的LF-NMR检测条件,即:TR=2000ms,τ=250μs,EchoCount=6000个,检测体积2.5mL,检测温度50℃。并应用建立的方法对多种地沟油样品进行了检测。结果表明,基于油样的LFNMR弛豫特性,可有效区分8种固态油样和10种液态地沟油,检测正确识别率可达75%和100%,有效避免了假阳性,且S21峰比例面积可有效反映样品的掺杂梯度变化,说明了该方法对固态和液态地沟油也具有较好的识别能力,在后期油脂品质检测应用中具有较好的可行性。
The effects of the LF-NMR instrument parameters,detection temperature and volume on the stability and reproducibility of oils' relaxometry characteristics results had been investigated with the taken soybean oil,palm oil and lard as the samples. The results indicated that good stability and reproducibility could be guaranteed if choosing the following parameters,such as TR=2000ms,τ=250μs,EchoCount=6000,and before the measurement,a sample of 2.5mL should be stabilized at 50℃. Then the method was employed to discriminate 8 solid oil samples,10 liquid hogwash oil samples. The result indicated that the proposed methodology was a useful tool to authenticate the hogwash oils,and the correct recognition rate was 75% and100%,respectively,and the false positive rate had been effectively avoided. Meanwhile,the difference of S21 peak area could reflect the adulterated ratio,which means that. The developed method had a good possibility to be used to assess the oil quality in the future.
The effects of the LF-NMR instrument parameters,detection temperature and volume on the stability and reproducibility of oils' relaxometry characteristics results had been investigated with the taken soybean oil,palm oil and lard as the samples. The results indicated that good stability and reproducibility could be guaranteed if choosing the following parameters,such as TR=2000ms,τ=250μs,EchoCount=6000,and before the measurement,a sample of 2.5mL should be stabilized at 50℃. Then the method was employed to discriminate 8 solid oil samples,10 liquid hogwash oil samples. The result indicated that the proposed methodology was a useful tool to authenticate the hogwash oils,and the correct recognition rate was 75% and100%,respectively,and the false positive rate had been effectively avoided. Meanwhile,the difference of S21 peak area could reflect the adulterated ratio,which means that. The developed method had a good possibility to be used to assess the oil quality in the future.
引文
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[2]Blümich B,Perlo J,Casanova F.Mobile single-sided NMR.Progress in Nuclear Magnetic Resonance Spectroscopy[J].2008,52(4):197-269.
[3]Brondum J,Munck L,Henckel P,et al.Prediction of waterholding capacity and composition of porcine meat by comparative spectroscopy[J].Meat Science,2000,55(2):177-185.
[4]Pitombo R N M,Lima G A.Nuclear magnetic resonance and water activity in measuring the water mobility in Pintato fish[J].Journal of Food Engineering,2003,58(1):59-66.
[5]Mazzanti G,Mudge E M,Anom E Y.In situ Rheo-NMR measurements of solid fat content[J].J Am Oil Chem Soc,2008,85(5):405-412.
[6]Hui Y H.贝雷:油脂化学与工艺学[M].北京:中国轻工业出版社,2001:121-122.
[7]Martina H,Hariette H,Heinz-Dieter I.Determination of total polar parts with new methods for the quality survey of frying fats and oils[J].Talanta,1998,47:447-454.
[8]王永巍.低场核磁共振技术在餐饮废油快速检测中的应用研究[D].上海:上海理工大学,2012.
[9]史然,王欣,刘宝林,等.大豆油煎炸过程理化指标与LFNMR弛豫特性的相关性研究[J].分析测试学报,2013,32(6):653-660.
[10]王乐,黎勇,胡建华,等.核磁共振法鉴别食用植物油掺伪餐饮业废油脂[J].中国油脂,2008,33(10):75-77.
[11]周凝,刘宝林,王欣,等.米糠毛油掺伪食用植物油的低场核磁共振检测[J].食品发酵与工业,2011,37(3):177-181.
[12]Lucas T,Ray D L,Barey P,et al.NMR assessment of ice cream:Effect of formulation on liquid and solid fat[J].International Dairy Journal,2005,15:1225:1233.
[13]史然,王欣,刘宝林,等.油脂低场核磁(LF-NMR)检测参数的优化实验[J].分析测试学报,2012,31(11):1365-1372.
[14]高汉宾,张振芳.核磁共振原理与实验方法[M].武汉:武汉大学出版社,2008:118-136.
[15]Chaland B,Mariette F,Machal P,et al.1H nuclear magnetic resonance relaxometric characterization of fat and water states in soft and hard cheese[J].Journal of Dairy Research,2000,67:609-618.
[16]Botlan D L,Fourel I H.A novel approach to the analysis of fats by low resolution NMR spectroscopy:application to milk and vegetable fats[J].Analysis,1994,22:108-113.