固相萃取-气相色谱法测定腌肉中5种生物胺
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摘要
采用固相萃取-气相色谱法测定腌肉中酪胺、组胺、精胺、亚精胺和β-苯乙胺等5种生物胺的含量。腌肉样品用50g·L~(-1)三氯乙酸溶液提取,强阳离子交换固相萃取柱净化。用Agilent DB-1701色谱柱(30m×0.25mm,0.25μm)分离,氮磷检测器检测。5种生物胺的质量浓度均在1.0~50.0mg·L~(-1)内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为0.12~0.32 mg·kg~(-1)。以空白样品为基体进行加标回收试验,所得回收率为78.0%~96.8%,测定值的相对标准偏差(n=6)为2.2%~7.1%。
GC was applied to the determination of 5 bioamines,i.e.tyramine,histamine,spermine,spermidine and phenylethylamine in bacon with solid phase extraction.The bacon sample was extracted with 50 g·L~(-1) trichloroacetic acid solution and purified by SCX solid phase extraction column.The analytes were separated on Agilent DB-1701 chromatographic column(30 m×0.25 mm,0.25μm)and detected by NPD.Linear relationships between values of peak area and mass concentration of the 5 bioamines were all kept in the same range of 1.0-50.0 mg·L~(-1),with detection limits(3 S/N)in the range of 0.12-0.32 mg·kg~(-1).On the base of blank sample,test for recovery was made by standard addition method.Values of recovery found were in the range of 78.0%-96.8%,with RSD′s(n=6)in the range of 2.2%-7.1%.
GC was applied to the determination of 5 bioamines,i.e.tyramine,histamine,spermine,spermidine and phenylethylamine in bacon with solid phase extraction.The bacon sample was extracted with 50 g·L~(-1) trichloroacetic acid solution and purified by SCX solid phase extraction column.The analytes were separated on Agilent DB-1701 chromatographic column(30 m×0.25 mm,0.25μm)and detected by NPD.Linear relationships between values of peak area and mass concentration of the 5 bioamines were all kept in the same range of 1.0-50.0 mg·L~(-1),with detection limits(3 S/N)in the range of 0.12-0.32 mg·kg~(-1).On the base of blank sample,test for recovery was made by standard addition method.Values of recovery found were in the range of 78.0%-96.8%,with RSD′s(n=6)in the range of 2.2%-7.1%.
引文
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[7]吴云辉,周爽,徐敦明.非衍生化液相色谱-串联质谱法测定动物源性食品中8种生物胺[J].色谱,2013,31(2):111-116.
[8]马明,沈稢,张峥,等.气固顶空-气相色谱法测定纺织品中N,N-二甲基甲酰胺与N,N-二甲基乙酰胺[J].理化检验-化学分册,2015,51(1):18-21.
[9]郑捷,李素,赵冰,等.固相萃取-高效液相色谱法测定羊肉风干肠中生物胺[J].食品工业,2015(3):286-289.
[2]REDRUELLO B,LADERO V,DEL RIO B,et al.A UHPLC method for the simultaneous analysis of biogenic amines,amino acids and ammonium ions in beer[J].Food Chemistry,2017,217:117-124.
[3]温永柱,范文来,徐岩.GC-MS法定性白酒中的多种生物胺[J].酿酒,2013(1):38-41.
[4]王树庆,范维江,李成凤.肉及肉制品中的生物胺[J].食品研究与开发,2016(24):203-206.
[5]GB 5009.208-2016食品安全国家标准食品中生物胺的测定[S].
[6]乔成栋,宋平顺,严祥,等.5种生物胺的毛细管胶束电动色谱分离[J].分析化学,2007,35(1):95-98.
[7]吴云辉,周爽,徐敦明.非衍生化液相色谱-串联质谱法测定动物源性食品中8种生物胺[J].色谱,2013,31(2):111-116.
[8]马明,沈稢,张峥,等.气固顶空-气相色谱法测定纺织品中N,N-二甲基甲酰胺与N,N-二甲基乙酰胺[J].理化检验-化学分册,2015,51(1):18-21.
[9]郑捷,李素,赵冰,等.固相萃取-高效液相色谱法测定羊肉风干肠中生物胺[J].食品工业,2015(3):286-289.