[Determination of two derivatives of cyanide in biomaterials by headspacegas gas chromatography mass spectrometry].

Objective: To establish a method for determination of two derivatives of cyanide in biomaterials by headspace gas chromatography mass spectrometry. Methods: In February 2024, blood and urine samples were placed in headspace sampling vials. Phosphoric acid, or phosphoric acid and chloramine T solution, was added respectively to derivatize cyanide into hydrogen cyanide or cyanogen chloride. After equilibrating at 80°C for 15 minutes, headspace sampling was performed. The samples were separated by a GS-GasPro chromatographic column and determined by gas chromatography-mass spectrometry in selected ion monitoring (SIM) mode. Qualitative analysis was conducted using both retention time and the ratio of characteristic ions, and quantitative analysis was carried out by the external standard method. Results: The correlation coefficients (r) for the two derivatives was 0.9992 and 0.9984, respectively. The detection limits was 0.10 μg/ml and 0.05 μg/ml, respectively. The recoveries ranged from 73.7% to 98.4%, with precision (RSD) ranging from 3.3% to 14.2%. Conclusion: The method offers the advantages of simple operation, precise quantification, high qualitative reliability, and high sensitivity, making it suitable for cyanide detection in biological materials.