二苯并18-冠-6修饰碳糊电极差分脉冲伏安法测定胡萝卜中的铅

Irdhawati Irdhawati, Ayu Jyostosya Yotirani Arya Wijana, Emmy Sahara, Manuntun Manurung
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摘要

本研究利用二苯并18-冠-6对碳糊电极(CPE)进行修饰,测定胡萝卜中铅的含量。这种电极修饰的目的是为了提高测量的灵敏度。优化参数为扫描速率、碳糊中二苯并18-冠-6的组成、支撑电解质。通过确定线性浓度范围、检出限(LoD)、定量限(LoQ)、重复性、选择性和回收率来验证测量结果。在最佳测定条件下,应用改性CPE (CPE- dbc)测定胡萝卜中的铅。得到了碳糊中冠醚的最佳浓度为0.8%,CPE扫描速率从15 mV/s提高到20 mV/s,以H2SO4溶液为支撑电解质的最佳测量条件。CPE的线性浓度范围为5-100µg/L, CPE- dbc的线性浓度范围为5-2000µg/L。CPE测得的LoD和LoQ分别为0.3575µg/L和0.3583µg/L, CPE- dbc测得的LoD和LoQ分别为0.1265µg/L和0.1266µg/L。CPE和CPE- dbc具有较好的精度,Horwitz比值分别为0.2231和0.2183,均小于2。标准溶液和样品溶液的铅回收率为(88,97±2,76)%。溶液中Cu、Cd和Na的存在对Pb的测量没有干扰。胡萝卜样品中Pb的浓度为(18423±0.0002)mg/kg,高于SNI No. 7387:2009规定的0.5 mg/kg的可接受浓度。
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Carbon Paste Electrode Modified by Dibenzo 18-crown-6 for the Determination of Pb in Carrot Using Differential Pulse Voltammetry
In this research, the modification of carbon paste electrode (CPE) using dibenzo 18-crown-6 was carried out to detect Pb level in carrot. The purpose of this electrode modification is to increase the sensitivity of the measurement. The optimized parameters were scan rate, composition of dibenzo 18-crown-6 in carbon paste, and supporting electrolyte. Measurements were validated by determining the linear concentration range, detection limit (LoD), quantification limit (LoQ), repeatability, selectivity, and recovery. At the best measurement conditions, the modified CPE (CPE-Dbc) was applied to determine Pb in carrot. The optimum measurements conditions were obtained the optimum concentration of crown ether in carbon paste was 0.8%, the scan rate using CPE at 15 mV/s, increased to 20 mV/s, and H2SO4 solution as supporting electrolyte. The linear concentration was found in the range of 5-100 µg/L using CPE and became wider to 5-2000 µg/L using CPE-Dbc. The values of LoD and LoQ measurement using CPE were 0,3575 µg/L and 0,3583 µg/L, and decreased to 0,1265 µg/L and 0,1266 µg/L using CPE-Dbc. CPE and CPE-Dbc had good precision with Horwitz ratio values were 0,2231 and 0,2183, which is smaller than two. The percentage of recovery of Pb in the mixture of standard and sample solutions was (88,97 ± 2,76)%. The presence of Cu, Cd and Na in the solution did not interfere the measurement of Pb. The concentration of Pb in carrot sample was (1,8423 ± 0,0002) mg/kg, which was higher than the acceptable concentration according to SNI No. 7387:2009, which is 0,5 mg/kg.
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