連續式氫化物生成系統配合感應耦合電漿原子放射分析儀(HG-ICP-AES)測定食品中硒含量之研究

Determination of Selenium in Food by Continuous Hydride Generation Inductively Coupled Plasma Atomic Emission Spectrometry

楊筱冬(Shiau-Dune Yang) ； 呂淑芳(Shu-Fang Lu) ； 傅偉光(Wei-Guang Fu)

《臺灣農業化學與食品科學》 42卷6期 (2004/12) Pp. 397-403

https://doi.org/10.6578/TJACFS.2004.051

摘要

本研究採用連續式氫化物生成系統感應耦合電漿原子放射分析儀(HG-ICP-AES)配合微波消化前處理方式測定食品中硒含量，內容包括氫化物生成系統之試驗條件探討，如消化液濃度、還原劑濃度、載流酸濃度及載流氣體流速等，並研究過渡元素及其他會產生氫化物之元素，在測定過程產生的干擾影響；在選定的試驗條件下，儀器偵測極限及方法偵測極限分別約為 05ng/mL此及20ng/g，銅離子的干擾問題可藉由L-半胱胺酸遮蔽劑(masking agent)的加入而改善，最後，藉由三種分別購自加拿大國家研究委員會(NRCC)及美國國家標準與技術研究院(NIST)之驗證參考物質(CRM)之測定結果而確認本方法之準確度，並進而估算其量測不確定度，且其回收率可達97.8-106.9%，偏差係數(CVs)介於1.3-4.6％。此外，本方法之優點是在相同試驗條件下，能同步進行硒與汞之分析，由於可有效縮短分析時間，故適用於大量樣品之例行分析。

關鍵字

硒 ； 氫化物生成系統 ； 感應耦合電漿原子放射分析法 ； 儀器偵測極限 ； 驗證參考物質 ； 量測不確定度

並列摘要

A continuous hydride generation inductively coupled plasma atomic emission spectrometric method (HG-ICP-AES) was developed for determining total selenium in food which was microwave digested. The experimental conditions such as digestion acid concentration, reducing agent concentration, carrier acid concentration, and flow rate of argon carrier gas were optimized. Interferences of testing results due to transition elements and other elements that can be converted to hydride forms were also investigated. Under optimized conditions, the instrument and method detection limit of the proposed method were 0.5 ng/mL and 20 ng/g, respectively. L-cysteine hydrochloride monohydrate was used to mask the interferences from copper ions. The method validation was carried out by testing three certified reference materials (CRM5) obtained from the National Research Council Canada (NRCC) and National Institute of Standards Technology (NIST). The results were all in excellent agreement with the certified values and the associated measurement uncertainties were also evaluated. Recoveries by the method ranged from 97.8 to 106.9%, with coefficients of variation (CVs) of 1.3-4.6%. Furthermore, this method can simultaneously determine selenium and mercury and the results showed its suitability for selenium determination in food, especially for routine analysis.

並列關鍵字

Selenium ； Hydride generation ； Inductively coupled plasma-atomic emission spectrometry ； Instrument detection limit ； Method detection limit ； Certified reference material ； Measurement uncertainty