氢化物原子荧光光谱法测定酱油中微量铅的方法研究

建立了一种快速、高效的QuEChERS-高效液相色谱-质谱联用法（QuEChERS-HPLC-MS/MS）测定谷类杂粮制品中脱氧雪腐镰刀菌烯醇（DON）、3-乙酰脱氧雪腐镰刀菌烯醇（3-ADON）、15-乙酰脱氧雪腐镰刀菌烯醇（15-ADON）和玉米赤霉烯酮（ZON）共4种真菌毒素。样品前处理采用乙腈-水溶剂提取，经Florisil+C18+无水硫酸镁净化后检测。以0.10%甲酸-乙腈作为流动相，在质谱检测器的多反应监测模式下进行分析。结果表明，4种真菌毒素在各自的线性范围内线性关系良好，相关系数R2均大于0.999，回收率在85.1%～102.0%，相对标准偏差（RSD）为2.11%～6.22%。该方法具有前处理简单、净化效果好、灵敏度高和检测速度快的优点，适用于谷类杂粮制品中DON、3-ADON、15-ADON 和ZON的分析和定量检测。

Methodology research on determination of trace lead in soy sauce by hydride atomic fluorescence spectrometry

A hydride atomic fluorescence spectrometric method for the determination of lead in soy sauce was established. Meanwhile, the precision and accuracy of the method were tested using soy sauce as samples, and the uncertainty of the blind sample for the verification of soy sauce ability was analyzed. The results showed that there was a linear relationship between the content of lead in the range of 0-100.00 ng/ml, the correlation coefficient (R) was 0.999 8, the detection limit of the method was 0.74 μg/L, the limit of quantitation was 2.22 μg/L, the relative standard deviation (RSD) of the precision test results was 1.16%-4.48%, and the recovery was 93.3%-106.6%. The uncertainty results of the two blind samples were (0.940±0.092) mg/L and (0.460±0.035) mg/L, respectively, and the results of competency verification were satisfactory. The results showed that lead in soy sauce samples was measured by hydride atomic fluorescence spectrometry, and the analytical quality control was adopted by quality control procedures for water quality analysis, ensuring experimental result error can be controlled in the permitted range and obtaining the highly reliable analytical results.