Λεπτομέρειες βιβλιογραφικής εγγραφής
| Τίτλος: |
CaCl2抑制-微波消解-原子荧光光谱法测定水果中痕量硒. (Chinese) |
| Alternate Title: |
Determination of Trace Selenium in Fruits by Atomic Fluorescence Spectrometry with Calcium Chloride Inhibition-Microwave Digestion. (English) |
| Συγγραφείς: |
吕, 静, 赵, 娜娜, 孟, 宁 |
| Πηγή: |
Chinese Journal of Inorganic Analytical Chemistry / Zhongguo Wuji Fenxi Huaxue; Sep2026, Vol. 16 Issue 9, p1794-1802, 9p |
| Θεματικοί όροι: |
Calcium chloride, Atomic fluorescence spectroscopy, Trace element analysis, Fruit composition, Scientific method, Volatization |
| Abstract (English): |
To effectively inhibit the volatile loss of selenium during the digestion process and reduce the systematic deviation of measurement results，this study selected formaldehyde，cuprous reagent，and calcium ions as candidate inhibitors. Through controlled experiments，the optimal type of inhibitor and its suitable concentration were screened. Meanwhile，key experimental parameters such as sample weight，digestion acid dosage，and microwave digestion temperature and time were systematically investigated. As a result，an analytical method for the determination of selenium content in fruits using microwave digestion coupled with atomic fluorescence spectrometry was established. The research results show that CaCl2，as an auxiliary additive in the digestion system，can effectively suppress the volatilization loss of selenium elements during the digestion process，significantly improving the accuracy and stability of trace selenium element determination results in the sample. The optimal measurement procedure for this experiment is as follows：accurately weigh 0.8 g of the sample，place it in a polytetrafluoroethylene digestion tank，add 2 mL of nitric acid （HNO3），2 mL of hydrogen peroxide （H2O2），and 6 mL of 0.02 µg/L CaCl2 solution in sequence，shake and mix well，and let it stand for 15 minutes；Subsequently，place the digestion tank into a microwave digestion apparatus and continue digestion at 80 ℃ for 25 minutes. After the digestion tank has cooled to room temperature，transfer it to a 120 ℃ acid analyzer until the characteristic white smoke of nitric acid completely disappears. Then slowly add 5 mL of 6 mol/L hydrochloric acid solution to the system，continue heating until dissolved，and finally dilute to 25 mL in a centrifuge tube. The method showed a good linear relationship in the concentration range of 0-40 µg/L，with a correlation coefficient （r） of 0.999 8. The limit of detection （LOD） was 0.029 µg/L，and the limit of quantification （LOQ） was 0.096 µg/L. Results from spiked recovery experiments at three levels （high，medium，and low） demonstrated recoveries ranging from 96.7% to 104%，with relative standard deviations （RSD） between 3.1% and 6.8%. This indicates that the method has excellent accuracy and precision，meeting the requirements for the precise detection of selenium in fruits. The application of this method to the actual determination of selenium content in 6 types of common fruits and 4 types of selenium-enriched fruits further verified its technical characteristics，including simple operation，accurate and reliable results，low detection limit，and excellent reproducibility. Therefore，this method is suitable for the batch detection of selenium content in fruit samples. 1） The reagents that inhibit the volatilization of selenium （Se） during digestion were screened out. 2） The pretreatment conditions such as sample weight，digestion acid dosage，microwave digestion time and temperature were optimized. 3） The applicability of the method was verified through experimental parameters such as limit of detection，limit of quantification，precision and accuracy. [ABSTRACT FROM AUTHOR] |
| Abstract (Chinese): |
为有效抑制消解过程中硒（Se）的挥发损失，降低测定结果的系统偏差。本研究选取甲醛、铜试剂、钙离子等作为候选抑制剂，通过对照实验筛选出最优抑制剂种类及适配浓度，同时系统考察称样量、消解酸用量、微波消解温度与时间等关键实验参数，建立了微波消解-原子荧光光谱法测定水果中硒含量的分析方法。该方法的最优实验条件确定为：以6 mL 0.02 µg/L CaCl2作为硒挥发抑制剂，样品称样量控制为0.8 g，消解体系采用4 mL HNO3-H2O2混合酸（体积比1∶1），微波消解温度为80 ℃，消解时间为25 min。该方法在0~40 µg/L表现出良好的线性关系，相关系数r=0.9998；方法检出限（LOD）为0.029 µg/L，定量限（LOQ）为0.096 µg/L。高中低三水平加标回收实验结果显示，回收率处于96.7%~104%，相对标准偏差（RSD）为3.1%~6.8%，表明该方法具备优良的准确度与精密度，可满足水果中硒含量的精准检测需求。将该方法应用于6种普通水果及4种富硒水果的硒含量实际测定，进一步验证了其操作简便、结果准确可靠、检出限低、重现性优良的技术特性，可适用于水果样品中硒含量的批量检测工作。 1） 筛选出消解过程中抑制硒（Se）挥发的试剂。 2） 优化了称样量、消解酸用量、微波消解时间与温度等前处理条件。 3） 通过检出限、定量限、精密度、准确度等实验参数验证了方法的适用性。 [ABSTRACT FROM AUTHOR] |
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| Βάση Δεδομένων: |
Complementary Index |