食品与发酵工业 >

2023 , Vol. 49 >Issue 14: 265 - 271

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.032871

分析与检测

微型氢化物发生原子荧光仪简便快速测定稻米中痕量镉

  • 李咸宇 ,
  • 罗明标 ,
  • 王为民 ,
  • 程雪萌 ,
  • 曾凯 ,
  • 董云雅 ,
  • 杨梅
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  • 1(东华理工大学 江西省合成化学重点实验室,江西 南昌,330013)
    2(国家环境保护重金属污染监测重点实验室,湖南 长沙,410019)
    3(重庆民泰新农业科技发展集团有限公司,重庆,400060)
硕士研究生(罗明标教授为通信作者, E-mail:mbluoecut555@126.com)

收稿日期: 2022-07-06

  修回日期: 2022-09-07

  网络出版日期: 2023-08-30

基金资助

国家环境保护重金属污染监测重点实验室基金(SKLMHM202109)

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Simple and rapid determination of trace cadmium in rice by miniature hydride generation atomic fluorescence spectrometry

  • LI Xianyu ,
  • LUO Mingbiao ,
  • WANG Weimin ,
  • CHENG Xuemeng ,
  • ZENG Kai ,
  • DONG Yunya ,
  • YANG Mei
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  • 1(Jiangxi Province Key Laboratory of Synthetic Chemistry, East China University of Technology, Nanchang 330013, China)
    2(State Environmental Protection Key Laboratory of Monitoring for Heavy Metal Pollutants, Changsha 410019, China)
    3(Chongqing Mintai New Agrotech Development Group Co.Ltd., Chongqing 400060, China)

Received date: 2022-07-06

  Revised date: 2022-09-07

  Online published: 2023-08-30

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摘要

基于自主研发的微型氢化物发生原子荧光仪,建立超声辅助稀酸浸提法简单、快速、准确地测定稻米中痕量镉。通过比较超声、离心、振荡、静置4种辅助浸提方式的稳定性,得到最佳辅助浸提方式;通过单因素实验考察了超声辅助稀酸浸提法中超声时间、超声功率、盐酸浓度、硫脲浓度、镉增敏剂浓度等对镉提取的影响,得到最佳浸提条件。结果表明,超声辅助浸提方式最佳,稳定性最好。最佳浸提条件为:超声时间10 min、超声功率80%、盐酸体积分数4%、硫脲质量浓度5.0 g/L、镉增敏剂质量浓度2.5 g/L。优化后,镉在0.05~0.25 ng/mL范围内线性良好,相关系数为0.999 8,方法检出限为0.000 61 mg/kg,加标回收率为93.3%~106.7%,相对标准偏差为1.62%~4.06%。采用大米标准物质GSB-1和GSB-22进行方法验证,结果准确可靠。与传统方法对比,该方法前处理简单、耗时短、测定准确,适用于稻米中痕量镉的测定。

关键词： 自主研发; 微型氢化物发生原子荧光仪; 快速; 镉; 稻米; 超声

本文引用格式

李咸宇 , 罗明标 , 王为民 , 程雪萌 , 曾凯 , 董云雅 , 杨梅 . 微型氢化物发生原子荧光仪简便快速测定稻米中痕量镉[J]. 食品与发酵工业, 2023 , 49(14) : 265 -271 . DOI: 10.13995/j.cnki.11-1802/ts.032871

Abstract

An ultrasound-assisted dilute acid extraction method for the simple, rapid and accurate determination of trace cadmium (Cd) in rice was established based on the self-developed miniature hydride generation atomic fluorescence spectrometer. The best auxiliary extraction way was obtained by comparing the stability of four auxiliary extraction ways, including ultrasonication, centrifugation, shaking, and resting. The effects of ultrasonic time, ultrasonic power, hydrochloric acid concentration, thiourea concentration, and cadmium sensitizer concentration on the extraction of cadmium were investigated by single-factor experiments to obtain the optimal extraction conditions. Results showed that ultrasound-assisted extraction had the best way and stability. The optimal extraction conditions were as follows: sonication time of 10 min, sonication power of 80%, hydrochloric acid concentration of 4% (volume ratio), thiourea concentration of 5.0 g/L, and cadmium sensitizer concentration of 2.5 g/L. After optimization, the linearity of Cd was good in the range of 0.05-0.25 ng/mL, and the correlation coefficient was 0.999 8. The detection limit of the method was 0.000 61 mg/kg, the recovery rate was 93.3%-106.7%, and the relative standard deviation was 1.62%-4.06%. The method was verified by rice standard substances GSB-1 and GSB-22, and the results were accurate and reliable. Compared with the traditional method, the method has simple pretreatment, short time consumption, and accurate determination, and is suitable for the determination of trace cadmium in rice.

Key words： independent development; miniature hydride generation atomic fluorescence spectrometer; quick; cadmium; rice; ultrasonic

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