LC-MS/MS method development and validation for quantitative analyses of 2-aminothiazoline-4-carboxylic acid – a new cyanide exposure marker in post mortem blood

Giebułtowicz, Joanna; Ruzycka-Ayoush, Monika; Fudalej, Marcin; Krajewski, Paweł; Wroczyński, Piotr

doi:10.1016/j.talanta.2015.12.076

Cited by 23 publications

(23 citation statements)

References 25 publications

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“…The endogenous and exogenous levels of CN and ATCA in the human blood are presented in Table 3 . 10 , 15 , 16 , 28 , 34 − 36 It became apparent that the present methods can be applied to the concentration ranges of fire incidents and CN poisoning and are satisfactory for forensic purposes. The raw data of the calibrants and QC samples are presented in Tables S2 and S3 .…”

Section: Resultsmentioning

confidence: 92%

“…In comparison with several earlier reports ( Table 2 ), the LLOD and LLOQ of the present methods were slightly higher. 8 , 15 , 27 − 32 However, sufficient sensitivity for practical use was obtained because PESI exhibited high ionization efficiency like nano-ESI, 33 even without analyte extraction. The endogenous and exogenous levels of CN and ATCA in the human blood are presented in Table 3 .…”

Section: Resultsmentioning

confidence: 99%

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RECiQ: A Rapid and Easy Method for Determining Cyanide Intoxication by Cyanide and 2-Aminothiazoline-4-carboxylic Acid Quantification in the Human Blood Using Probe Electrospray Ionization Tandem Mass Spectrometry

et al. 2020

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In this study, we developed a rapid and easy method to determine cyanide (CN) intoxication by quantification of CN and 2-aminothiazoline-4-carboxylic acid (ATCA), which is a new and reliable indicator of CN exposure, in the human blood using probe electrospray ionization tandem mass spectrometry (PESI/MS/MS) named RECiQ. For CN, we applied the previously reported one-pot derivatization method using 2,3-naphthalenedialdehyde and taurine, which can directly derivatize CN in the blood. The analytical conditions of the CN derivatization were optimized as a 10 min reaction time at room temperature. In contrast, ATCA could be directly detected in the blood by PESI/MS/MS. We developed quantitative methods for the derivatized CN and ATCA using an internal standard method and validated them using quality control samples, demonstrating that the linearities of each calibration curve were greater than 0.995, and intra- and interday precisions and accuracies were 5.1–15 and 1.1–14%, respectively. Moreover, the lower limit of detections for CN and ATCA were 42 and 43 ng/mL, respectively. Finally, we applied RECiQ to three postmortem blood specimens obtained from victims of fire incidents, which resulted in the successful quantification of CN and ATCA in all samples. As PESI/MS/MS can be completed within 0.5 min, and the sample volume requirement of RECiQ is only 2 μL of blood, these methods are useful not only for the rapid determination of CN exposure but also for the estimation of the CN intoxication levels during an autopsy.

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Section: Resultsmentioning

confidence: 92%

Section: Resultsmentioning

confidence: 99%

RECiQ: A Rapid and Easy Method for Determining Cyanide Intoxication by Cyanide and 2-Aminothiazoline-4-carboxylic Acid Quantification in the Human Blood Using Probe Electrospray Ionization Tandem Mass Spectrometry

et al. 2020

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“…Although LLE offered good accuracy and sensitivity with an LOD of 0.43 ng/mL, derivatization of interference compounds (secondary amino acids) was required to remove interference peaks [ 72 ]. It was applied to human blood and revealed that ATCA concentrations in blood from a cyanide-poisoned person were approximately four-fold higher than those from non-poisoned persons.…”

Section: Analytical Methods For Carboxylic Acids In Biological Sammentioning

confidence: 99%

“…The concentrations of six α-keto acids were between 1.55 and 316 pmol per 106 cells and LODs were within 1.3 and 5.4 nM, being three-fold higher than that of OPD. Quantification entailing OPD derivatization and fluorescence detection has been reported by several groups, wherein LODs were between 18 nM and 1 µM [70][71][72]. DMB was developed to improve the sensitivity of fluorescence detection, and has a structure similar to that of OPD.…”

Section: α-Keto Acids and Their Metabolitesmentioning

confidence: 99%

Liquid-Chromatographic Methods for Carboxylic Acids in Biological Samples

et al. 2020

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Carboxyl-bearing low-molecular-weight compounds such as keto acids, fatty acids, and other organic acids are involved in a myriad of metabolic pathways owing to their high polarity and solubility in biological fluids. Various disease areas such as cancer, myeloid leukemia, heart disease, liver disease, and lifestyle diseases (obesity and diabetes) were found to be related to certain metabolic pathways and changes in the concentrations of the compounds involved in those pathways. Therefore, the quantification of such compounds provides useful information pertaining to diagnosis, pathological conditions, and disease mechanisms, spurring the development of numerous analytical methods for this purpose. This review article addresses analytical methods for the quantification of carboxylic acids, which were classified into fatty acids, tricarboxylic acid cycle and glycolysis-related compounds, amino acid metabolites, perfluorinated carboxylic acids, α-keto acids and their metabolites, thiazole-containing carboxylic acids, and miscellaneous, in biological samples from 2000 to date. Methods involving liquid chromatography coupled with ultraviolet, fluorescence, mass spectrometry, and electrochemical detection were summarized.

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“…Most methodologies of preparing samples for the determination of total cyanide content consist of adding sodium hydroxide to pH greater than 12, which results in trapping the volatile forms of cyanides and then in carrying out the distillation operation. Spectrophotometric techniques [9–11], which have been used for many years, are now mostly replaced by chromatographic ones (both GC [12, 13] and LC [14]), which are characterized by higher selectivity and sensitivity, while capillary electrophoresis [15] is rarely used.…”

Section: Introductionmentioning

confidence: 99%

Development of an Analytical Protocol for Determination of Cyanide in Human Biological Samples Based on Application of Ion Chromatography with Pulsed Amperometric Detection

Jaszczak

Ruman

Narkowicz

et al. 2017

Journal of Analytical Methods in Chemistry

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A simple and accurate ion chromatography (IC) method with pulsed amperometric detection (PAD) was proposed for the determination of cyanide ion in urine, sweat, and saliva samples. The sample pretreatment relies on alkaline digestion and application of Dionex OnGuard II H cartridge. Under the optimized conditions, the method showed good linearity in the range of 1–100 μg/L for urine, 5–100 μg/L for saliva, and 3–100 μg/L for sweat samples with determination coefficients (R) > 0.992. Low detection limits (LODs) in the range of 1.8 μg/L, 5.1 μg/L, and 5.8 μg/L for urine, saliva, and sweat samples, respectively, and good repeatability (CV < 3%, n = 3) were obtained. The proposed method has been successfully applied to the analysis of human biological samples.

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LC-MS/MS method development and validation for quantitative analyses of 2-aminothiazoline-4-carboxylic acid – a new cyanide exposure marker in post mortem blood

Cited by 23 publications

References 25 publications

RECiQ: A Rapid and Easy Method for Determining Cyanide Intoxication by Cyanide and 2-Aminothiazoline-4-carboxylic Acid Quantification in the Human Blood Using Probe Electrospray Ionization Tandem Mass Spectrometry

RECiQ: A Rapid and Easy Method for Determining Cyanide Intoxication by Cyanide and 2-Aminothiazoline-4-carboxylic Acid Quantification in the Human Blood Using Probe Electrospray Ionization Tandem Mass Spectrometry

Liquid-Chromatographic Methods for Carboxylic Acids in Biological Samples

Development of an Analytical Protocol for Determination of Cyanide in Human Biological Samples Based on Application of Ion Chromatography with Pulsed Amperometric Detection

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