Study on simultaneous determination of zinc and gluconate in nutritional supplements by CE-C4D

Huyen Trang Luu Thi
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Abstract

Nutritional supplements providing bioavailable essential minerals, such as zinc (Zn) and magnesium (Mg), in forms of absorbable salts (e.g., gluconate, stearate, lactate, etc.) have been widely used. However, it should be noted that alongside these supplements, some excipients, including inorganic salts like zinc sulfate and magnesium sulfate, are frequently employed in pharmaceutical and nutraceutical products. Conventional analytical methods for total metal contents could not distinguish actual concentrations of bioavailable forms, suggesting the need for simultaneous analysis of both these essential minerals and their corresponding salts. In this study, we applied the capillary electrophoresis with capacitively coupled contactless conductivity detection (CE-C4D) method to simultaneously measure zinc and gluconate in nutritional supplements. The optimal analytical parameters comprise: (1) 10 mM Tris/Ace electrolyte solution at pH 5.0; (2) silica capillary with an internal diameter of 50 μm and an effective length of 30 cm; (3) separation voltage of +15 kV; (4) hydrodynamic injection mode with siphoning technique at 10 cm height and injection time of 20 s. With these conditions, limit of detections of 1.0 mg/L for zinc and 1.5 mg/L for gluconate were achieved. The method has good repeatability (RSD < 3%) and good recovery (89-103% for zinc and 88-107% for gluconate). The validated method was applied to determine zinc and gluconate concentrations in three commercially available nutritional supplement samples. To ascertain the validity of the results, cross-validation was performed using the high-performance liquid chromatography with photodiode array detection (HPLCPDA) for gluconate and the inductively coupled plasma optical emission spectrometry (ICPOES) for zinc, thereby reinforcing the reliability of the CE-C4D method.
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利用 CE-C4D 同时测定营养补充剂中锌和葡萄糖酸盐的研究
营养补充剂以可吸收盐(如葡萄糖酸盐、硬脂酸盐、乳酸盐等)的形式提供生物可利用的必需矿物质,如锌(Zn)和镁(Mg),已被广泛使用。不过,需要注意的是,除了这些补充剂,一些辅料,包括硫酸锌和硫酸镁等无机盐,也经常被用于药品和营养保健品中。传统的总金属含量分析方法无法区分生物可利用形式的实际浓度,这表明需要同时分析这些必需矿物质及其相应的盐类。在这项研究中,我们采用毛细管电泳与电容耦合非接触电导检测法(CE-C4D)同时测定营养补充剂中的锌和葡萄糖酸盐。最佳分析参数包括:(1)10 mM Tris/Ace 电解质溶液,pH 5.0;(2)硅胶毛细管,内径 50 μm,有效长度 30 cm;(3)分离电压 +15 kV;(4)流体动力进样模式,虹吸技术,进样高度 10 cm,进样时间 20 s。该方法重复性好(RSD < 3%),回收率高(锌回收率为 89-103%,葡萄糖酸回收率为 88-107%)。应用该方法测定了三种市售营养补充剂样品中锌和葡萄糖酸盐的浓度。为了确定结果的有效性,使用高效液相色谱-光电二极管阵列检测法(HPLCPDA)和电感耦合等离子体光发射光谱法(ICPOES)对葡萄糖酸盐和锌进行了交叉验证,从而加强了CE-C4D方法的可靠性。
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