Development of a dual-chamber derivatization method for the determination of cyanide in sodium nitroprusside and its preparation via HS-GC-ECD

开发了一种双室衍生化方法,用于测定硝普钠中的氰化物,并通过顶空-气相色谱-电子捕获检测器(HS-GC-ECD)进行制备。

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Abstract

The acute toxicity of cyanide and its pharmaceutical residues has fueled interest in the development of analytical methods for its determination, particularly for sodium nitroprusside (SNP), a widely used vasodilator with potential cyanide residues. In this study, a dual-chamber derivatization bottle was designed to establish an interconnected gas environment, thereby facilitating chloramine T-mediated cyanide conversion to cyanogen chloride (CNCl) without direct contact with SNP. Subsequent determination of the analytes was undertaken using a headspace-gas chromatography-electron capture detector (HS-GC-ECD). The challenges of analyzing cyanide and the rapid degradation of SNP were addressed simultaneously. The method was subjected to rigorous validation, encompassing specificity, linearity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, precision, and robustness. The validation process revealed a notable degree of linearity within the range of 0.012-1.56 μg/mL, with a LOQ of 12.0 ng/mL. The method was found to be both accurate and precise, thus satisfying the requisite criteria. This method facilitates reliable cyanide monitoring in degradation-prone pharmaceuticals.

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