目的: 建立准确度高,适用性强的胶体果胶铋胶囊的含量测定方法。方法: 紫外-可见分光光度法以10%抗坏血酸溶液-20%碘化钾溶液-1 mol·L-1硝酸溶液(2∶5∶1)为显色剂,测定波长463 nm;电位滴定法以光度电极为指示电极,测定波长590 nm,以二甲酚橙为指示剂,用0.05 mol·L-1乙二胺四醋酸二钠滴定液进行滴定;原子吸收分光光度法以223.1 nm为测定波长。结果: 紫外-可见分光光度法、电位滴定法与原子吸收分光光度法分别在2~20 μg·mL-1、30~70 mg、5~30 μg·mL-1范围内线性良好,平均回收率分别为100.0%(RSD=0.40%)、100.4%(RSD=0.49%)和100.3%(RSD=0.51%)。18批次样品按上述3种方法测定,含量范围分别为97.1%~104.8%、97.4%~105.0%和97.5%~104.8%。建立的3种方法均能准确测定胶体果胶铋胶囊含量,测定结果之间无统计学差异。结论: 考虑仪器的普适性及方法的灵敏度,紫外-可见分光光度法更适用于胶体果胶铋胶囊的含量测定。
Objective: To establish a method with high accuracy and applicability for the content determination of colloidal bismuth pectin capsules. Methods: UV-Vis spectrophotometry used 10% ascorbic acid solution-20% potassium iodide solution-1 mol·L-1 nitric acid solution(2∶5∶1) as chromogenic agent, and the determination wavelength was 463 nm. Potentiometric titration was carried out using photometric electrode as indicator electrode at 590 nm, with xylenol orange as an indicator and 0.05 mol·L-1 EDTA as titration. The wavelength was measured at 223.1 nm by atomic absorption spectrophotometry(AAS). Results: The good linear relationships were found in the range of 2-20 μg·mL-1,30-70 mg and 5-30 μg·mL-1 for UV-Vis spectrophotometry, potentiometric titration and AAS, respectively. The average recoveries were 100.0% (RSD=0.40%), 100.4% (RSD=0.49%) and 100.3%(RSD=0.51%). Eighteen batches of samples were determined by the above three methods, the content ranges were 97.1%-104.8%, 97.4%-105.0% and 97.5%-104.8%, respectively. The three established methods could accurately determine the content of colloidal pectin bismuth capsules, and the results showed no significant difference. Conclusion: Considering the universality of the instrument and the sensitivity of method, UV-Vis spectrophotometry is more suitable for the content determination of colloidal bismuth pectin capsules.
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