Dataset Information

Forensic analysis using ultra-high-performance liquid chromatography-tandem mass spectrometry with solid-phase extraction of α-solanine and α-chaconine in whole blood.

ABSTRACT:

Purpose

The potato glycoalkaloids (PGAs), α-solanine and α-chaconine can exert adverse effects on human health when consumed in excess. This study aimed to investigate the optimal extraction method for the quantitative analysis of PGAs in whole blood by using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) and to apply this validated method to postmortem blood.

Methods

A total of 200 µL of human whole blood was prepared for PGA extraction. For validation, a solid-phase extraction (SPE) using Oasis^® PRiME HLB, in which extraction could be performed in three simple steps (sample loading, washing, and elution) was used, with no need for both conditioning and equilibration of columns for sample preparation.

Results

In this method, the limit of detection and the lower limit of quantification (LLOQ) of both α-solanine and α-chaconine were 1 and 2 µg/L, respectively. The calibration curves of the two compounds were obtained with good linearity in the range of 2-100 µg/L. The recovery rates at the LLOQ of α-solanine and α-chaconine were ≥ 91.8% and ≥ 85.9%, respectively. The validation data (intra- and inter-day combined) for accuracy ranged from 93.5 to 106.6% for α-solanine and from 93.9 to 107.7% for α-chaconine. This validated method was successfully applied to one forensic autopsy case, and the concentrations of α-solanine and α-chaconine in the postmortem cardiac blood were 45.1 and 35.5 µg/L, respectively.

Conclusions

This validated UHPLC-MS/MS with SPE for quantitative analysis of PGAs could be useful in forensic toxicology.

SUBMITTER: Nara A

PROVIDER: S-EPMC6314998 | biostudies-literature | 2019

REPOSITORIES: biostudies-literature

ACCESS DATA

Publications

Forensic analysis using ultra-high-performance liquid chromatography-tandem mass spectrometry with solid-phase extraction of α-solanine and α-chaconine in whole blood.

Nara Akina A Saka Kanju K Yamada Chiho C Kodama Takanori T Takagi Tetsuya T

Forensic toxicology 20181119 1

<h4>Purpose</h4>The potato glycoalkaloids (PGAs), α-solanine and α-chaconine can exert adverse effects on human health when consumed in excess. This study aimed to investigate the optimal extraction method for the quantitative analysis of PGAs in whole blood by using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) and to apply this validated method to postmortem blood.<h4>Methods</h4>A total of 200 µL of human whole blood was prepared for PGA extraction. For v ...[more]

PMID: 30636987

Similar Datasets

Project description:Monoaromatic hydrocarbons (MAHs) such as benzene, toluene, and xylene are important anthropogenic pollutants in the urban atmosphere. The detection of urinary MAH metabolites are included in human biomonitoring programs in several countries, including Canada, the United States, Italy, and Germany, because their evaluation is vital to monitor the exposure of humans to MAHs. To this end, herein, a method was developed for the determination of seven MAH metabolites through ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). An aliquot of 0.5 mL urine was fortified with an isotopic labeled internal standard solution before being hydrolyzed by 40 μL of 6 mol/L HCl solution, followed by extraction using a 96-well EVOLUTE®EXPRESS ABN solid-phase extraction plate. The samples were washed with 1.0 mL of methanol-water (10∶90, v/v) and eluted with 1.0 mL methanol. The eluate was diluted four times with water prior to use in instrumental analysis. Chromatographic separation was achieved using an ACQUITY UPLC HSS T3 column (100 mm×2.1 mm, 1.8 μm), with gradient elution using 0.1% formic acid as mobile phase A and methanol as mobile phase B. The detection of seven analytes was performed using a triple-quadrupole mass spectrometer equipped with a negative electrospray ionization source in the multiple reaction monitoring mode. The linear ranges of the seven analytes varied from 0.1-20 μg/L to 2.5-500 mg/L, with correlation coefficients greater than 0.995. The method detection limits were 1.5, 0.02, 0.1, 900, 0.6, and 4 μg/L for trans,trans-muconic acid (MU), S-phenylmercapturic acid (PMA), S-benzylmercapturic acid (BMA), hippuric acid (HA), 2-methyl hippuric acid (2MHA), and 3-methyl hippuric acid (3MHA)+4-methyl hippuric acid (4MHA), respectively. The limits of quantification were 5, 0.05, 0.4, 3000, 2, and 12 μg/L for MU, PMA, BMA, HA, 2MHA, and 3MHA+4MHA, respectively. The method was verified by spiking urine samples at three different concentration levels, with recovery rates ranging from 84% to 123%. The intra- and inter-day precisions were 1.8%-8.6% and 1.9%-21.4%, respectively. The extraction efficiencies were 68%-99%, and the matrix effects ranged from -11% to -87%. The urine samples obtained from the German external quality assessment scheme (round 65) were used to assess the accuracy of this method. Both high and low concentrations of MU, PMA, HA, and methyl hippuric acid were within the tolerance range. All analytes in the urine samples were found to be stable for up to seven days at room temperature (20 ℃, absence of light), with less than 15% change in concentration. Analytes in urine samples were found to be stable for at least 42 d at 4 ℃ and -20 ℃, or for six freeze-thaw cycles and up to 72 h in an autosampler (8 ℃). The method was applied to the analysis of 16 non-smokers' and 16 smokers' urine samples. The detection rates of MU, BMA, HA, and 2MHA were 100% in both non-smokers' and smokers' urine samples. PMA was detected in 75% non-smokers' and 100% smokers' urine samples. 3MHA+4MHA was detected in 81% non-smokers' urine and in all smokers' urine samples. Statistical differences were found for MU, PMA, 2MHA, and 3MHA+4MHA between the two groups (p<0.001). The established method has good robustness and can provide reliable results. The experiments were carried out in a high-throughput manner with large sample sizes, owing to the small sample volume, and allowed the successful detection of the seven MAH metabolites in human urine.

Dataset Information

Forensic analysis using ultra-high-performance liquid chromatography-tandem mass spectrometry with solid-phase extraction of α-solanine and α-chaconine in whole blood.

Purpose

Methods

Results

Conclusions

Publications

Forensic analysis using ultra-high-performance liquid chromatography-tandem mass spectrometry with solid-phase extraction of α-solanine and α-chaconine in whole blood.

Similar Datasets

OmicsDI is part of the ELIXIR infrastructure

Tweets