微敞开体系快速石墨消解-原子荧光法测定食品及土壤中的硒

李蕾; 苏园; 陈楚国; 文典; 赵沛华; 邓腾灏博; 杜瑞英

doi:10.7524/j.issn.0254-6108.2019080704

环境化学

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李蕾, 苏园, 陈楚国, 文典, 赵沛华, 邓腾灏博, 杜瑞英. 微敞开体系快速石墨消解-原子荧光法测定食品及土壤中的硒[J]. 环境化学, 2020, (4): 1098-1104. doi: 10.7524/j.issn.0254-6108.2019080704

引用本文:

LI Lei, SU Yuan, CHEN Chuguo, WEN Dian, ZHAO Peihua, DENG Tenghaobo, DU Ruiying. Fast determination of selenium in food and soils by micro-open graphite digestion-atomic fluorescence spectrometry[J]. Environmental Chemistry, 2020, (4): 1098-1104. doi: 10.7524/j.issn.0254-6108.2019080704

Citation:

LI Lei, SU Yuan, CHEN Chuguo, WEN Dian, ZHAO Peihua, DENG Tenghaobo, DU Ruiying. Fast determination of selenium in food and soils by micro-open graphite digestion-atomic fluorescence spectrometry[J]. Environmental Chemistry, 2020, (4): 1098-1104. doi: 10.7524/j.issn.0254-6108.2019080704

微敞开体系快速石墨消解-原子荧光法测定食品及土壤中的硒

1. 广东省农业科学院农产品公共监测中心, 广州, 510640;
2. 农业农村部农产品质量安全检测与评价重点实验室, 广州, 510640;
3. 广东农科监测科技有限公司, 广州, 510640

通讯作者: 杜瑞英, E-mail: duruiying@163.com

基金项目:
国家重点研发计划（2018YFD0800700）和国家自然科学基金（41701369）资助.

Fast determination of selenium in food and soils by micro-open graphite digestion-atomic fluorescence spectrometry

1. Public Monitoring Center for Agro-product of Guangdong Academy of Agricultural Sciences, Guangzhou, 510640, China;
2. Key Laboratory of Testing and Evaluation for Agro-Product Safety and Quality, Ministry of Agriculture, Guangzhou, 510640, China;
3. Guangdong Agricultural Science Monitoring Technology Co., Ltd., Guangzhou, 510640, China

Corresponding author: DU Ruiying, duruiying@163.com

Fund Project: Supported by National Key R&D Program of China (2018YFD0800700) and the National Natural Science Foundation of China (41701369).

摘要: 本文采用一种新型消化管，优化和构建了一套快速高通量测定食品及土壤中硒的微敞开体系石墨消解-原子荧光光谱法体系.主要对比了不同消化温度、不同加酸量对样品消化时间的影响，并进一步优化了消解后硒还原的相关步骤.结果表明，这种新型的消化管可以保证高温消解过程中硒测定的准确度及精密度.在200 ℃的消化温度下，食品及土壤的消化时间可以分别在3.0 h及5.5 h内完成，中途无需加酸；使用本方法，食品中硒的检出限为0.003 μg·kg^-1，平均加标回收率为96.3%，精密度（RSD）在1.36%—3.28%之间；土壤中硒的检出限为0.007 μg·kg^-1，平均加标回收率为91.8%—98.3%，精密度在0.28%—0.64%之间.在0—20 μg·L^-1范围内，标准曲线具有良好的线性（r=0.9997）.本实验构建的硒检测体系具有步骤少、用时短、精密度高等特点，可以应用于快速高通量的食品及土壤样品检测.
- 石墨消解 /
- 原子荧光光谱 /
- 消化管 /
- 硒 /
- 食品 /
- 土壤
Abstract: The mass production of selenium (Se)-enriched products in recent years has greatly increased the demand for Se determination in food and soils. In this paper, a novel high-throughput method for temperature-controlled graphite digestion-atomic fluorescence spectrometry for the determination of Se in food and soil was established and optimized by using a new type of digestive tube. The effects of different digestion temperatures and different acid additions on digestion time were compared, and the relevant steps of Se reduction after digestion were also optimized. The results showed that this new type of digestive tube could ensure the accuracy and precision of Se determination during high temperature digestion. At the digestion temperature of 200 ℃, the digestion of food and soils can be finished in 3.0 h and 5.5 h, respectively, without any acid supplement. Based on this method, the detection limit of Se in food was 0.003 μg·kg^-1, the average recovery rate was 96.3%, and the precision (RSD) was between 1.36% and 3.28%. While the detection limit in soil was 0.007 mg·kg^-1, the average recovery rate was 91.8%—98.3%, and the RSD was between 0.28%—0.64%. The standard curve demonstrated a good linearity (r=0.9997) in the range of 0—20 μg·L^-1. Compared to other methods, the Se determination method established in this research had the characteristics of simplified steps, short digestive time and high precision, which would be a significant choice for the fast detection of large number of food and soil samples.
- graphite digestion /
- atomic fluorescence spectrometry /
- digestive tube /
- selenium /
- food /
- soil

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微敞开体系快速石墨消解-原子荧光法测定食品及土壤中的硒

通讯作者: 杜瑞英, E-mail: duruiying@163.com

1. 广东省农业科学院农产品公共监测中心, 广州, 510640;
2. 农业农村部农产品质量安全检测与评价重点实验室, 广州, 510640;
3. 广东农科监测科技有限公司, 广州, 510640

收稿日期: 2019-08-07

基金项目:

国家重点研发计划（2018YFD0800700）和国家自然科学基金（41701369）资助.

关键词:

摘要: 本文采用一种新型消化管，优化和构建了一套快速高通量测定食品及土壤中硒的微敞开体系石墨消解-原子荧光光谱法体系.主要对比了不同消化温度、不同加酸量对样品消化时间的影响，并进一步优化了消解后硒还原的相关步骤.结果表明，这种新型的消化管可以保证高温消解过程中硒测定的准确度及精密度.在200 ℃的消化温度下，食品及土壤的消化时间可以分别在3.0 h及5.5 h内完成，中途无需加酸；使用本方法，食品中硒的检出限为0.003 μg·kg^-1，平均加标回收率为96.3%，精密度（RSD）在1.36%—3.28%之间；土壤中硒的检出限为0.007 μg·kg^-1，平均加标回收率为91.8%—98.3%，精密度在0.28%—0.64%之间.在0—20 μg·L^-1范围内，标准曲线具有良好的线性（r=0.9997）.本实验构建的硒检测体系具有步骤少、用时短、精密度高等特点，可以应用于快速高通量的食品及土壤样品检测.

English Abstract

Fast determination of selenium in food and soils by micro-open graphite digestion-atomic fluorescence spectrometry

Corresponding author: DU Ruiying, duruiying@163.com

1. Public Monitoring Center for Agro-product of Guangdong Academy of Agricultural Sciences, Guangzhou, 510640, China;
2. Key Laboratory of Testing and Evaluation for Agro-Product Safety and Quality, Ministry of Agriculture, Guangzhou, 510640, China;
3. Guangdong Agricultural Science Monitoring Technology Co., Ltd., Guangzhou, 510640, China

Received Date: 2019-08-07

Fund Project: Supported by National Key R&D Program of China (2018YFD0800700) and the National Natural Science Foundation of China (41701369).

Keywords:

Abstract: The mass production of selenium (Se)-enriched products in recent years has greatly increased the demand for Se determination in food and soils. In this paper, a novel high-throughput method for temperature-controlled graphite digestion-atomic fluorescence spectrometry for the determination of Se in food and soil was established and optimized by using a new type of digestive tube. The effects of different digestion temperatures and different acid additions on digestion time were compared, and the relevant steps of Se reduction after digestion were also optimized. The results showed that this new type of digestive tube could ensure the accuracy and precision of Se determination during high temperature digestion. At the digestion temperature of 200 ℃, the digestion of food and soils can be finished in 3.0 h and 5.5 h, respectively, without any acid supplement. Based on this method, the detection limit of Se in food was 0.003 μg·kg^-1, the average recovery rate was 96.3%, and the precision (RSD) was between 1.36% and 3.28%. While the detection limit in soil was 0.007 mg·kg^-1, the average recovery rate was 91.8%—98.3%, and the RSD was between 0.28%—0.64%. The standard curve demonstrated a good linearity (r=0.9997) in the range of 0—20 μg·L^-1. Compared to other methods, the Se determination method established in this research had the characteristics of simplified steps, short digestive time and high precision, which would be a significant choice for the fast detection of large number of food and soil samples.