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正相高效液相色谱法测定腌腊肉制品中磷脂酰胆碱氢过氧化物的含量 被引量:1

Determination of Phosphatidylcholine Hydroperoxide in Dry Cured Meat Products by Normal-Phase High Performance Liquid Chromatography
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摘要 采用正相高效液相色谱法对腌腊肉制品中的磷脂酰胆碱氢过氧化物(PC-OOH)进行检测。腌腊肉制品中的PC-OOH用氯仿-甲醇(2∶1,V/V)提取,以合成的C16∶0/18∶2 PC-OOH为标样,采用正相高效液相色谱-紫外法进行检测。色谱柱:Lichrosorb Si60(250 mm×4.0 mm,5μm);流动相:A为水,B为正己烷-异丙醇(3∶2,V/V),采用梯度洗脱;流速:1 m L/min;柱温:30℃;检测波长:234 nm。结果表明:C16∶0/18∶2 PC-OOH在20~600 nmol/m L范围内呈现良好的线性关系(R2=0.999 9),检出限为5.8 nmol/m L,定量限为19.4 nmol/m L,不同水平的平均回收率为79.4%~91.9%。实际样品分析显示,农家腊肠A、B和火腿中方样品中PC-OOH的含量比较高,为92.4、106.4 nmol/g和102.5 nmol/g,烟熏肉中未检出PC-OOH。本实验建立的分析方法简便快捷、具有较好的灵敏度和可靠性,可用于腌腊肉制品中PC-OOH的定量分析。 A normal-phase high-performance liquid chromatographic(HPLC) method was established to determine phosphatidylcholine monohydroperoxide(PC-OOH) in dry cured meat products. The PC-OOH in dry cured meat samples was extracted with chloroform/methanol(2:1, V/V), followed by determination by normal-phase HPLC connected to a photo-diode array detector(HPLC-PAD) with synthetic C16:0/18:2 PC-OOH as the standard. The chromatographic conditions were established using a Lichrosorb Si60 column(250 mm × 4.0 mm, 5 μm) with a mobile phase consisting of water and n-hexane/isopropanol(3:2, V/V) in gradient elution at a flow rate of 1.0 m L/min. The detection wavelength was set at 234 nm. Results indicated that the linearity ranged from 20 to 600 nmol/m L(R^2 = 0.999 9), and the limits of detection(LOD) and limits of quantification(LOQ) were 5.8 nmol/m L and 19.4 nmol/m L, respectively. The recoveries from spiked samples at concentration levels of 32–240 nmol/g were in the range of 79.4%–91.9%. The contents of PC-OOH in farm-made sausage A, B and Chinese ham samples were 92.4, 106.4 and 102.5 nmol/g, respectively, while PC-OOH in smoked meat was not detected. This method proved to be of high maneuverability, excellent sensitivity and high accuracy, and could be used for quantitative analysis of PC-OOH in dry cured meat samples.
出处 《食品科学》 EI CAS CSCD 北大核心 2016年第14期154-159,共6页 Food Science
基金 国家自然科学基金青年科学基金项目(31401560) 江苏省农业科技自主创新资金项目(CX(13)3081)
关键词 腌腊肉制品 1-棕榈酰-2-亚油酰-磷脂酰胆碱 氢过氧化物 正相高效液相色谱法 dry cured meat 1-palmitoyl-2-linoleoyl-phosphatidylcholine hydroperoxide normal-phase HPLC
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参考文献28

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