Development of a preparation method to produce a single sample that can be applied to both LC–MS/MS and GC–MS for the screening of postmortem specimens

doi:10.1016/J.LEGALMED.2016.06.005

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Development of a preparation method to produce a single sample that can be applied to both LC–MS/MS and GC–MS for the screening of postmortem specimens

Journal Article•DOI•

Development of a preparation method to produce a single sample that can be applied to both LC–MS/MS and GC–MS for the screening of postmortem specimens

Kenji Hara¹, Brian Waters¹, Natsuki Ikematsu¹, Tomoko Tokuyasu¹, Hiroshi Fujii¹, Mio Takayama¹, Aya Matsusue¹, Masayuki Kashiwagi¹, Shin-ichi Kubo¹ - Show less +5 more•Institutions (1)

Fukuoka University¹

01 Jul 2016-Legal Medicine (Elsevier)-Vol. 21, pp 85-92

TL;DR: Simple and efficient extraction methods have been developed for the screening of a wide array of drugs in postmortem autopsy specimens that could easily be incorporated into a forensic laboratory's daily routine for screening many different compounds from postmortem samples.

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About: This article is published in Legal Medicine.The article was published on 2016-07-01. It has received 17 citations till now.

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Journal Article•DOI•

Determination of 12 commonly found compounds in DUID cases in whole blood using fully automated supported liquid extraction and UHPLC-MS/MS.

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Lena Kristoffersen¹, Marit Langødegård¹, K.I. Gaare¹, I. Amundsen¹, M.N. Terland¹, Dag Helge Strand¹ - Show less +2 more•Institutions (1)

Oslo University Hospital¹

01 Sep 2018-Journal of Chromatography B

TL;DR: This is the first automated 96-well SLE UHPLC-MS/MS method developed for the simultaneous determination of these 12 compounds in whole blood covering the concentration ranges found in forensic samples and has proven to be robust and reliable.

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25 citations

Journal Article•DOI•

A report of novel psychoactive substances in forensic autopsy cases and a review of fatal cases in the literature

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Shin-ichi Kubo¹, Brian Waters¹, Kenji Hara¹, Tatsushige Fukunaga², Kazuya Ikematsu³ - Show less +1 more•Institutions (3)

Fukuoka University¹, Tokyo Metropolitan Government², Nagasaki University³

01 May 2017-Legal Medicine

13 citations

Journal Article•DOI•

A fast and simple approach for the quantification of 40 illicit drugs, medicines, and pesticides in blood and urine samples by UHPLC-MS/MS.

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Sarah Carobini Werner de Souza Eller Franco de Oliveira¹, Sarah Carobini Werner de Souza Eller Franco de Oliveira², Alexandre Dias Zucoloto², Carolina Dizioli Rodrigues de Oliveira, Edna M. M. Hernandez, Ligia Veras Gimenez Fruchtengarten, Tiago Franco de Oliveira¹, Mauricio Yonamine² - Show less +4 more•Institutions (2)

University of Health Sciences Antigua¹, University of São Paulo²

01 Jul 2019-Journal of Mass Spectrometry

TL;DR: The developed method was successfully applied to 320 real samples collected at the Poison Control Center of São Paulo and 89.1% have shown to be positive for some of the analytes, confirming its applicability and importance to emergency toxicological analysis.

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Abstract: A fast and simple approach to overcome challenges in emergency toxicological analysis, using ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) has been developed, for the detection of analytes in blood and urine samples from the following drug classes: analgesics, benzodiazepines, antidepressants, anticonvulsants, drugs of abuse, and pesticides. These substances are relevant in the context of emergency toxicology in Brazil. The sample preparation procedure was relatively easy and fast to perform. The method was fully validated giving limits of in the range of 0.5 and 20 ng mL-1 for blood and urine samples. The intraday and interday precision and accuracy were considered adequate for all analytes once the relative standard deviation (RSD) (%) was lower than 20% for quality control (QC) low and lower than 15% for CQ medium and high. The developed method was successfully applied to 320 real samples collected at the Poison Control Center of Sao Paulo, and 89.1% have shown to be positive for some of the analytes. This confirms its applicability and importance to emergency toxicological analysis, and it could be very useful in both fields of clinical and forensic toxicology.

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12 citations

Journal Article•DOI•

Tissue Distribution of Suvorexant in Three Forensic Autopsy Cases.

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Brian Waters¹, Kenji Hara¹, Natsuki Ikematsu¹, Mio Takayama¹, Aya Matsusue¹, Masayuki Kashiwagi¹, Shin-ichi Kubo¹ - Show less +3 more•Institutions (1)

Fukuoka University¹

01 May 2018-Journal of Analytical Toxicology

TL;DR: This is the first instance of suvorexant being quantitated from actual autopsy cases and it is likely that this compound will be encountered more often by the forensic toxicology community going forward.

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Abstract: Suvorexant (Belsomra®) is a relatively new insomnia medication that has been available in USA and Japan since 2014. It is a dual orexin receptor antagonist that promotes sleep by inhibiting the binding of orexin neurons to the OX1R and OX2R receptors. In this report, we describe the detection and quantitation of suvorexant from the postmortem specimens of three separate autopsy cases handled by our department. Suvorexant was identified by fast gas chromatography/mass spectrometry during routine screening, and quantitated by a fully validated liquid chromatography-tandem mass spectroscopy method. Quantitation was achieved by positive electrospray ionization in the selected reaction monitoring mode. Monitored transitions were m/z 451 > 186 for quantitation and m/z 451 > 104 for qualification. To our knowledge, this is the first instance of suvorexant being quantitated from actual autopsy cases. It is likely that this compound will be encountered more often by the forensic toxicology community going forward.

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9 citations

Cites methods from "Development of a preparation method..."

...The preparation method for postmortem body fluid samples for the routine screening of drugs by fast GC-MS can be found in a previous report (12)....
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Journal Article•DOI•

Medical mass spectrometrist (MMS) training and certification: A key step to expanding routine clinical mass spectrometry usage in Japan

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Fumio Nomura¹, Toyofumi Nakanishi², Kazuo Igarashi, Seiji Yamaguchi³, Mitsutoshi Setou⁴, Toshimitsu Niwa⁵ - Show less +2 more•Institutions (5)

Chiba University¹, Osaka Medical College², Shimane University³, Hamamatsu University School of Medicine⁴, Shubun University⁵

01 Jan 2020-Clinical Mass Spectrometry

TL;DR: The adoption of MS-based assays for routine testing in clinical chemistry is very slow and it is believed that they will play significant roles for expanding routine clinical MS usage in Japan.

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4 citations

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References

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Journal Article•DOI•

Systematic and comprehensive strategy for reducing matrix effects in LC/MS/MS analyses

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Erin E. Chambers¹, Diane M. Wagrowski-Diehl¹, Ziling Lu¹, Jeffrey R. Mazzeo¹•Institutions (1)

Waters Corporation¹

01 Jun 2007-Journal of Chromatography B

TL;DR: The combination of polymeric mixed-mode SPE, the appropriate mobile phase pH and UPLC technology provides significant advantages for reducing matrix effects resulting from plasma matrix components and in improving the ruggedness and sensitivity of bioanalytical methods.

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680 citations

"Development of a preparation method..." refers background or methods in this paper

...The presence of these compounds may have a great influence on GC–MS results, with interfering peaks and background noise [6]....
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...The overall flow of both extraction methods involved the following processes: 1) sample pretreatment (urea removal [8]); 2) protein removal and extraction; 3) main lipid removal [6]; 4) salting out and removal of amino acid derivatives; and 5) ion exchange (removal of salts) [3]....
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Journal Article•DOI•

Optimization of protein precipitation based upon effectiveness of protein removal and ionization effect in liquid chromatography-tandem mass spectrometry.

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Cara Polson, Pratibha Sarkar, Bev Incledon, Vanaja Raguvaran, Russell P. Grant - Show less +1 more

05 Mar 2003-Journal of Chromatography B

TL;DR: Four categories of protein precipitation techniques were tested in plasma using spectrophotometry to assess protein removal efficiency across a range of volumes, species and lots and acetonitrile, trichloroacetic acid and zinc sulfate were found to be optimal at removing protein in their categories.

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613 citations

"Development of a preparation method..." refers methods in this paper

...Many methods for the extraction of drugs have been developed, including simple protein precipitation (PPE) [1], liquid-liquid extraction (LLE) [2], and solid-phase extraction (SPE) [3]....
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Journal Article•DOI•

High-throughput quantitative bioanalysis by LC/MS/MS.

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Mohammed Jemal¹•Institutions (1)

Bristol-Myers Squibb¹

01 Oct 2000-Biomedical Chromatography

TL;DR: This review article discusses the most recent significant advances in the sample preparation and mass spectrometry aspects of high-throughput bioanalysis by LC/MS/MS for the quantitation of drugs, metabolites and endogenous biomolecules in biological matrices.

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Abstract: This review article discusses the most recent significant advances in the sample preparation and mass spectrometry aspects of high-throughput bioanalysis by LC/MS/MS for the quantitation of drugs, metabolites and endogenous biomolecules in biological matrices. The introduction and implementation of automated 96-well extraction has brought about high-throughput approaches to the biological sample preparation techniques of solid-phase extraction, liquid-liquid extraction and protein precipitation. The fast-flow on-line extraction technique is a different high-throughput approach that has also significantly speeded up analysis by LC/MS/MS. The use of pierceable caps for biological tubes further enhances the analysis speed and improves the safety in handling biological samples. The need for adequate chromatographic separation in order to eliminate interferences due to metabolites and/or matrix effects in LC/MS/MS is discussed. To highlight our limited understanding of atmospheric pressure ionization mass spectrometry, results from recent investigations that appear to be counter-intuitive are presented. Looking ahead to the future, multiplexed LC/MS/MS systems and capillary LC are presented as areas that can bring about further improvements in analysis speed and sensitivity to quantitative bioanalysis by LC/MS/MS.

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352 citations

"Development of a preparation method..." refers background in this paper

...LC–MS/MS is amenable to certain compounds that suffer from thermal breakdown during GC–MS analysis, and for compounds that do not readily volatilize [5]....
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Book•

Liquid-Liquid Extraction

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Ruth Blumberg

01 Jul 1988

TL;DR: PreLab : Prepare a PreLab as you have for the last two experiments and do this exercise: Draw a flow diagram similar to that in Figure 6.15.10 for the substances 2,4, and 6.

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Abstract: PreLab : Prepare a PreLab as you have for the last two experiments and do this exercise: Draw a flow diagram similar to that in Figure 6.10 for the substances 2,4, and 6 shown in Figure 6.15.

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301 citations

Journal Article•DOI•

Recent developments in polymer-based sorbents for solid-phase extraction.

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Christian W. Huck¹, Guenther K. Bonn¹•Institutions (1)

University of Innsbruck¹

14 Jul 2000-Journal of Chromatography A

TL;DR: New polymer-based materials, chromatographic modes, experimental configurations are described and their advantages for a rapid sample preparation of certain classes of compounds with different functional groups are discussed and compared to silica-based sorbents.

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289 citations

"Development of a preparation method..." refers methods in this paper

...The overall flow of both extraction methods involved the following processes: 1) sample pretreatment (urea removal [8]); 2) protein removal and extraction; 3) main lipid removal [6]; 4) salting out and removal of amino acid derivatives; and 5) ion exchange (removal of salts) [3]....
[...]
...Many methods for the extraction of drugs have been developed, including simple protein precipitation (PPE) [1], liquid-liquid extraction (LLE) [2], and solid-phase extraction (SPE) [3]....
[...]
...Solid-phase extraction (SPE) is typically used in one of two ways, by retaining the analytes of interest on the SPE media and later eluting them, or by allowing the analytes to pass through the SPE media while trapping the matrix interferences and undesirable components [3]....
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