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

PurposeThe 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.MethodsA 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.ResultsIn 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.ConclusionsThis validated UHPLC–MS/MS with SPE for quantitative analysis of PGAs could be useful in forensic toxicology.Electronic supplementary materialThe online version of this article (10.1007/s11419-018-0452-7) contains supplementary material, which is available to authorized users.

Risk assessment of glycoalkaloids in feed and food, in particular in potatoes and potato‐derived products

“…Hossain et al (2015) reported LOQs for a-solanine and a-chaconine of 2 lg/L in potato extract, corresponding to 40 lg/kg in dehydrated potato powder. Nara et al (2019) reported an LOQ of 1 and 2 lg/L in whole blood for a-solanine and a-chaconine, respectively.…”

“…Combined with the high sensitivity of modern mass spectrometers, sample preparation and clean-up can often be minimised and simple dilution of extracts may be sufficient. Methods based on LC coupled to tandem mass spectrometry (LC-MS/MS) are often used for targeted analysis of GAs (Jandri c et al, 2011;Hossain et al, 2015;Nara et al, 2019), while methods using LC coupled to high resolution MS (LC-HRMS) or to Orbitrap MS (LC-Orbitrap-MS) are more commonly used for metabolomic studies and exploratory research (Moco et al, 2007;Caprioli et al, 2014). Hossain et al (2015) reported LOQs for a-solanine and a-chaconine of 2 lg/L in potato extract, corresponding to 40 lg/kg in dehydrated potato powder.…”

“…Nara et al. () reported an LOQ of 1 and 2 μg/L in whole blood for α‐solanine and α‐chaconine, respectively.…”

Easily Operable Quantification Method of 21 Plant-Derived Alkaloids in Human Serum by Automatic Sample Preparation and Liquid Chromatography–Tandem Mass Spectrometry

“…The concentrations of each glycoalkaloid in pooled human serum were 0.067 ± 0.013 ng/mL for α-solanine, 0.33 ± 0.11 ng/mL for α-chaconine, and 0.60 ± 0.17 ng/mL for solanidine (Table S5). The concentrations of these glycoalkaloids were significantly lower than those in the blood of glycoalkaloid poisoning cases in previous studies [ 29 , 32 ], suggesting that the glycoalkaloids detected in the pooled human serum used in this study would be derived from a daily diet. These results confirmed that our method could detect glycoalkaloids even at sub-ppb concentration levels.…”

Quantitative analysis of 17 hypoglycemic drugs in fingerprints using ultra‐high‐performance liquid chromatography/tandem hybrid triple quadrupole linear ion trap mass spectrometry

“…All the solutions were stored at À20 C in darkness when not in use. 27 Working standard solutions were prepared by serial diluting the mixed stock solutions with methanol and were stored at 4 C. A blank matrix of fingerprints was collected from healthy volunteers after they had provided informed consent, and the samples were screened for the 17 hypoglycemic drugs all of which were confirmed to be negative. Matrix-matched solutions were prepared by diluting the mixed stock solutions with the blank matrix and were stored at 4 C in the same way.…”