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Sensitive Detection of Cyanide in Urine by HPLC ESI–MS/MS Combined with Derivatization Pretreatment

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Abstract

The high toxicity and availability in industrial production have made cyanide a concern for clinical testing and forensic toxicological analysis. An efficient and accurate method for detecting cyanide in urine sample has been established. The process was carried out by a two-step derivatization reaction. The cyanide reacted with benzaldehyde to form a stable intermediate which reacted with heptafluorobutyryl chloride in the second step. The quantitative MS/MS transition of the cyanide derivative was m/z 330.2→m/z 303.4, and the qualitative MS/MS transition was m/z 330.2→m/z 185.2. The method had good linearity (r2 = 0.999 4) and covered the cyanide poisoning detection window (0.01–10 µg mL− 1), and the limit of detection was 3 ng mL− 1. At the same time, the method demonstrated good accuracy (recoveries = 92.7.0–102.0%) and precision (intra-day precision = 3.3–5.1%, inter-day precision = 4.4–5.3%). The complete derivatization reaction and detection time were controlled within 20 min and successfully applied in a lethal case of ingestion of potassium cyanide.

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Funding

This study was funded by National Natural Science Fund of China (81671864 and 81601644) and Research Item of Liaoning Provincial Natural Science Fund (20170541031).

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Authors and Affiliations

  1. School of Forensic Medicine, China Medical University, Shenyang, 110122, People’s Republic of China

    Huiya Yuan, Lina Gao, Enyu xu & Junting Liu

  2. College of Basic Medical Sciences, China Medical University, Shenyang, 110122, People’s Republic of China

    Guojie Liu

Authors
  1. Huiya Yuan
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  2. Guojie Liu
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  3. Lina Gao
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  4. Enyu xu
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  5. Junting Liu
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Corresponding author

Correspondence to Junting Liu.

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The authors declare that they have no conflict of interest.

Ethical approval

This study was approved by the Ethics Committee of China Medical University. The study was conducted under the supervision of the CMU Center of Medico-legal Investigation and obtained the consent of the relatives of the deceased.

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Yuan, H., Liu, G., Gao, L. et al. Sensitive Detection of Cyanide in Urine by HPLC ESI–MS/MS Combined with Derivatization Pretreatment. Chromatographia 82, 709–714 (2019). https://doi.org/10.1007/s10337-019-03698-w

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  • DOI: https://doi.org/10.1007/s10337-019-03698-w

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