食品科学
食品科學
식품과학
FOOD SCIENCE
2010年
4期
201-205
,共5页
气相色谱-质谱联用%三聚氰胺%三聚氰胺一酰胺%三聚氰胺二酰胺%三聚氰酸
氣相色譜-質譜聯用%三聚氰胺%三聚氰胺一酰胺%三聚氰胺二酰胺%三聚氰痠
기상색보-질보련용%삼취청알%삼취청알일선알%삼취청알이선알%삼취청산
GC-MS%melamine%ammeline%ammelide%cyanuric acid
建立一种简单、快速、准确同时测定大米蛋白粉中三聚氰胺及其类似物三聚氰酸、三聚氰胺一酰胺、三聚氰胺二酰胺的方法.样品经二乙胺-水-乙腈(1:4:5,V/V)超声提取30min后,提取液于70℃条件下氮气吹干,在吡啶介质中经甲基硅烷化衍生后采用气相色谱-质谱仪测定(内标法定量).此方法检测限为0.5mg/kg、线性相关系数(20～1000 μg/L范围内)不小于0.9989:当加标量为1.0～5.0mg/kg时,平均同收率为72.01%～96.45%、相对标准偏差不大于6.3%.此方法可用于大米蛋白粉中三聚氰酸及其类似物的检测.
建立一種簡單、快速、準確同時測定大米蛋白粉中三聚氰胺及其類似物三聚氰痠、三聚氰胺一酰胺、三聚氰胺二酰胺的方法.樣品經二乙胺-水-乙腈(1:4:5,V/V)超聲提取30min後,提取液于70℃條件下氮氣吹榦,在吡啶介質中經甲基硅烷化衍生後採用氣相色譜-質譜儀測定(內標法定量).此方法檢測限為0.5mg/kg、線性相關繫數(20～1000 μg/L範圍內)不小于0.9989:噹加標量為1.0～5.0mg/kg時,平均同收率為72.01%～96.45%、相對標準偏差不大于6.3%.此方法可用于大米蛋白粉中三聚氰痠及其類似物的檢測.
건립일충간단、쾌속、준학동시측정대미단백분중삼취청알급기유사물삼취청산、삼취청알일선알、삼취청알이선알적방법.양품경이을알-수-을정(1:4:5,V/V)초성제취30min후,제취액우70℃조건하담기취간,재필정개질중경갑기규완화연생후채용기상색보-질보의측정(내표법정량).차방법검측한위0.5mg/kg、선성상관계수(20～1000 μg/L범위내)불소우0.9989:당가표량위1.0～5.0mg/kg시,평균동수솔위72.01%～96.45%、상대표준편차불대우6.3%.차방법가용우대미단백분중삼취청산급기유사물적검측.
A GC-MS method was developed for the determination of melamine and its analogues in rice protein powder,like ammeline,ammelide and eyanurie acid.Samples were extracted with a mixture composed of diethylamine,water and acetonitrile (1:4:5,V/V)for 30 min,and the resulting extract was blown to dryness under dry nitrogen atmosphere at 70 ℃.Subsequently,the residue left was dissolved in pyridine and silylated for 40 min at 70 ℃ prior to GC-MS analysis.The internal standard method was used for quantification.Melamine and its analogues all exhibited a good linear curve over the concentration range of 20-1000 μg/L(r≥0.9989).The limit of detection(LOD)of the developed method was 0.5 mg/kg.Mean recoveries of melamine and its analogues at three spike levels of 1.0,2.0 mg/kg and 5.0 mg/kg were between 72.01%-96.45%,with relative standard deviations(RSDs)not more than 6.3%.These figures of merit of this method demonstrate its good applicability to the determination of melamine and its analogues in rice protein powder.
