Determination of Cr, Se, Ge, and V in Hypothyroidism Patients by Using Graphite Furnace Atomic Absorption Spectrometry and mixture matrix modification

Halah Hamid Hammadi
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Abstract

A simple, accurate and rapid method was developed for routine determination of trace elements in blood serum. The method based on the direct determination for Cr, Se, Ge, and V in hypothyroidism patients before therapy. By using atomic absorption spectrometry with graphite surface coated and uncoated pyrolysis GF-AAS, and a mixture of palladium nitrate and magnesium nitrate as the matrix modifier, with deuterium background correction and no sample pretreatment except dilution was necessary. This permitted direct determination hence the risk of sample contamination was reduced. Further, the use of graphite surface-coated GF-AAS decreased the ashing and atomization temperatures of Cr, Ge, and V to values that were lesser than the corresponding values obtained using uncoated pyrolysis GF-AAS, by 100°C; in case of Se, the atomization temperature decreased to a value that was 200°C lesser than that obtained using uncoated pyrolysis GF-AAS. A mixture of (3µL) palladium nitrate, and (2µL) magnesium nitrate was successfully applied to improve the sensitivity, reproducibility, recovery, limit of detection and the accuracy of the measurements. The correlation coefficients of the calibration curves of Cr, Se, Ge, and V were found to be (0.9999, 0.9999, 0.9995 and 0.9999) respectively, the relative standard deviation of the measurements for Cr, Se, Ge and V were (0.027, 0.075, 0.054 and 0.068) respectively. The statistical analysis of the acquired data showed acceptable accuracy. The analyses thus performed indicated that the levels of serum trace elements Cr, Se, Ge, and V in hypothyroidism patients were lower than those in the control group.
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石墨炉原子吸收光谱法和混合基体改性法测定甲状腺功能减退患者的Cr、Se、Ge和V
建立了一种简单、准确、快速的血清微量元素常规测定方法。该方法基于治疗前甲状腺功能减退患者的Cr、Se、Ge、V的直接测定。采用石墨表面包覆和未包覆热解GF-AAS原子吸收光谱法,以硝酸钯和硝酸镁的混合物为基体改性剂,进行氘背景校正,除稀释外无需样品前处理。这允许直接测定,因此降低了样品污染的风险。此外,使用石墨表面包覆的GF-AAS使Cr、Ge和V的灰化和雾化温度比使用未包覆的热解GF-AAS的相应温度低100℃;在Se的情况下,雾化温度下降到比未包覆热解GF-AAS低200℃。(3µL)硝酸钯和(2µL)硝酸镁的混合物被成功地应用于提高灵敏度、重现性、回收率、检出限和测量的准确性。结果表明,Cr、Se、Ge和V的校准曲线相关系数分别为(0.9999、0.9999、0.9995和0.9999),Cr、Se、Ge和V的相对标准偏差分别为(0.027、0.075、0.054和0.068)。对采集数据的统计分析显示出可接受的准确性。结果表明,甲减患者血清微量元素Cr、Se、Ge、V的含量低于对照组。
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