摘要
目的建立油条中铝含量的电感耦合等离子体质谱检测方法(ICP-MS)。方法用5 ml硝酸和2 ml过氧化氢为消解溶剂对样品进行微波消解,消解液蒸缩至1 ml左右,用纯水定容至50 ml,电感耦合等离子体质谱法进行定量检测。方法考察了酸度对响应值的影响,用1.0 ng/ml混合调谐液优化仪器工作条件,选用钪作为内标元素校正基体干扰和漂移。结果铝的质量浓度为0 mg/L^5.0 mg/L时,线性关系良好,线性回归方程为y=5 530x+62 184,相关系数(r)为0.999 3。方法的检出限为0.1μg/L。添加3种浓度水平的铝标准溶液测定方法的回收率,平均回收率为92.0%~102.0%,相对标准偏差为0.7%~3.2%。并应用该方法对油条样品中铝的含量进行了测定,发现15份样品中铝含量全部超标,含量为375 mg/kg^926 mg/kg。结论该方法灵敏度高、准确度好、检出限低、线性范围宽,适用于油条等面制食品中铝的测定。
Objective To develop a method for the determination of aluminum in fried bread stick by microwave digestion- inductively coupled plasma- mass spectrometry( ICP- MS). Methods The samples was conducted for microwave digestion with5 ml of nitris acid and 2 ml of hydroge peroxide. The digestion solution was evaporated to 1 ml and diluted to 50 ml with pure water,which was determined by ICP- MS. Effect of acidity was tested to response value and condition of instrument operation was optimized with 1. 0 ng/ml of mixed tune solution. Scandium was chosen as the internal standard,which was used to correct matrix interference and signal drifting. Results When aluminum concentration was within 0. 0 mg/L- 5. 0 mg/L,the linear relationship was good,and the linear regression equation was y = 5 530 x + 62 184,with correlation coefficient( r) = 0. 999 3.Detection limit of the method was 0. 1 μg/L. Recovery of the method was tested by addition of aluminum standard solution at 3concentration levels. The average recovery and the relative standard derivations of the method were within 92. 0%- 102. 0%and 0. 7%- 3. 2%. The developed method was applied to determine aluminum content in fried bread stick,with the concentration of aluminum in all 15 samples exceeding the standards within 375 mg/kg- 926 mg/kg. Conclusion The method shows high sensitivity,good accuracy,low detection limit,wide linear range,and is suitable for the determination of aluminum in wheaten food such as fried bread stick.
作者
迂君
高嵘
冯宇飞
YU Jun GAO Rong FENG Yu-fei(Shenyang Municipal Center for Disease Control and Prevention, Shenyang, Liaoning 110031, China)
出处
《中国卫生检验杂志》
CAS
2016年第20期2928-2929,2932,共3页
Chinese Journal of Health Laboratory Technology
关键词
微波消解
电感耦合等离子体质谱法
铝
油条
Microwave digestion
Inductively coupled plasma-mass spectrometry
Aluminum
Fried bread stick