投稿时间:2017-09-22      点此下载全文 HTML
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姜桦韬 中国农业科学院 烟草研究所, 山东 青岛 266101  
尤祥伟 中国农业科学院 烟草研究所, 山东 青岛 266101  
张广雨 中国农业科学院 烟草研究所, 山东 青岛 266101  
隋程程 中国农业科学院 烟草研究所, 山东 青岛 266101  
王秀国 中国农业科学院 烟草研究所, 山东 青岛 266101  
李义强 中国农业科学院 烟草研究所, 山东 青岛 266101 liyiqiang1008@163.com 
中文摘要:采用QuEChERS前处理与液相色谱-串联质谱(LC-MS/MS)技术,建立了糙米中氟唑环菌胺残留的分析方法。样品采用V(乙腈): V(水)=80:20混合溶液涡旋提取,经PSA分散固相萃取净化,LC-MS/MS测定,外标法定量。结果表明:在0.001~0.1 mg/L范围内,氟唑环菌胺的质量浓度与对应的峰面积间线性关系良好,R2 > 0.996。在0.004、0.01和0.1 mg/kg添加水平下,氟唑环菌胺在糙米中的回收率为83%~95%,相对标准偏差(RSD)为3.9%~12%。以最小添加浓度确定氟唑环菌胺在糙米中的定量限(LOQ)为0.004 mg/kg,远低于国际食品法典委员会规定的最大残留限量(MRL)0.01 mg/kg。所建方法操作简单、准确度和灵敏度高,可用于糙米中氟唑环菌胺残留的检测。对中国6个省(市)40个糙米样品进行检测,氟唑环菌胺的残留量均低于LOQ 0.004 mg/kg。膳食风险评估结果表明,氟唑环菌胺目前在中国水稻上使用对一般人群的的健康风险很低。
中文关键词:QuEChERS  液相色谱-串联质谱  糙米  氟唑环菌胺  残留
Determination of sedaxane in brown rice by QuEChERS-liquid chromatography-tandem mass spectrometry
Abstract:An analytical method for the determination of sedaxane residues in brown rice was established by QuEChERS and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with a mixture of acetonitrile and water (80/20, V/V), purified by dispersion solid phase extraction with PSA as sorbent, and quantified using LC-MS/MS by external standard method. The results showed that good linearity was obtained in the range from 0.001 to 0.1 mg/L, with R2 > 0.996. At the fortified levels of 0.004, 0.01 and 0.1 mg/kg, the recoveries of sedaxane in brown rice samples were 83%-95% with the relative standard deviations (RSD) of 3.9%-12%. The limit of quantitation (LOQ) was 0.004 mg/kg in brown rice samples, which was significantly lower than the maximum residue limit (MRL) of 0.01 mg/kg set by the Codex Alimentarius Commission. The proposed method is simple, accurate and sensitive. Hence, it could be used for the detection of sedaxane residues in brown rice. A market survey of 40 brown rice samples from 6 provinces was carried out, and the residual amount of sedaxane was less than 0.004 mg/kg in all samples. The dietary risk assessment showed that the use of sedaxane in rice was currently at a low risk in China.
Key words:QuEChERS  liquid chromatography-tandem mass spectrometry (LC-MS/MS)  brown rice  sedaxane  residue
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