摘要
应用固相萃取-高效液相-串联质谱(SPE-HPLC-MS/MS)建立6-苄基腺嘌呤(6-BA)在豆芽中残留的检测方法,并根据所建立的数学模型评定该方法测量不确定度的各分量。样品用0.1%乙酸乙腈提取,经Oasis MCX固相小柱净化,液相色谱-串联质谱测定,外标法定量。结果显示,豆芽样品中6-BA的含量为0.160 mg/kg时,其扩展不确定度为0.011 mg/kg(k=2),测定结果的表示式为(0.160±0.011)%,k=2。结果表明,测定结果的不确定度主要来源于回收率、标准溶液的配制及采用最小二乘法拟合标准工作曲线求得样品浓度过程。
A method for trace level analysis of 6- BA in bean- sprout by solid phase extraction / high performance liquid chromatography/tandem mass spectrometry (HPLC-MS/MS) was developed. The mathematical model was established and used to evaluate the uncertainty components of this method. The sample was extracted with 0.1% acetic acid acetonitrile di- rectly, and purified by Oasis MCX (SPE), then analyzed by using HPLC-MS/MS , and the quantization was carried out by the external standard method. The evaluation indicated that the expanded uncertainty was 0.011 mg/kg (k=2) when the 6- BA content in bean-sprout sample was 0.160 mg/kg, and the mathematical expression of the determination result of 6-BA content was (0,160 +0.011 )%, k=2. The results showed that the measurement uncertainty is mainly due to recovery rate, preparation process of standard solution and the least square fitting of the working curve.
出处
《福建分析测试》
CAS
2016年第3期19-23,共5页
Fujian Analysis & Testing
基金
厦门市科技计划项目(3502Z20132010)