Determination of lysergide in urine by high-performance liquid chromatography combined with electrospray ionisation mass spectrometry

White, Stephen; Catterick, Tim; Harrison, Mark E.; Johnston, Derek E.; Reed, G. D.; Webb, Kenneth S.

doi:10.1016/s0378-4347(96)00344-1

Cited by 25 publications

(5 citation statements)

References 16 publications

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“…When implementing a single quadrupole LC‐Q‐MS method to the analysis of LSD, MIPLA, and LAMPA, it was found that LSD (29.95 min) could be conveniently separated from MIPLA and LAMPA (30.52 min) but MIPLA and LAMPA could not be separated (Figure 6a) even after attempts to optimize the method and conditions further. LC‐based separations between LSD and LAMPA have been reported in the literature 8,10,14,17,37,60 . In some cases, the separation between LSD and LAMPA was unsuccessful under the conditions used 16 whereas other reports showed a partial overlap still suitable for differentiation 11–13,15 .…”

Section: Resultsmentioning

confidence: 99%

“…LC-based separations between LSD and LAMPA have been reported in the literature. 8,10,14,17,37,60 In some cases, the separation between LSD and LAMPA was unsuccessful under the conditions used 16 whereas other reports showed a partial overlap still suitable for differentiation. [11][12][13]15 Various other methods employing LAMPA as an internal standard have also been reported 36,42,61 with one method displaying partial overlap.…”

Section: Lc-msmentioning

confidence: 99%

“…These involved high‐performance liquid chromatography (HPLC), 8,10–17 gas chromatography (GC), 8,14–16,18–25 infrared spectroscopy (IR) (with or without coupling to a separation device), 7,11,15,21,24,26,27 nuclear magnetic resonance spectroscopy (NMR), 6,13,15 and other methods of separation, such as thin‐layer chromatography (TLC), 7,8,18 and capillary electrophoresis 28–32 . Furthermore, a variety of bioanalytical methods used for the detection of LSD included the use of LAMPA as an internal standard 33–44 . Compared to LSD and LAMPA, analytical studies involving the investigation of MIPLA are scarce 8,45 .…”

Section: Introductionmentioning

confidence: 99%

“…[28][29][30][31][32] Furthermore, a variety of bioanalytical methods used for the detection of LSD included the use of LAMPA as an internal standard. [33][34][35][36][37][38][39][40][41][42][43][44] Compared to LSD and LAMPA, analytical studies involving the investigation of MIPLA are scarce. 8,45 Recently, the detection of MIPLA in blotters seized in Japan was reported which involved the use of GCmass spectrometry (GC-MS), liquid chromatography (LC)-MS, and NMR analyses.…”

Section: Introductionmentioning

confidence: 99%

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Separating the wheat from the chaff: Observations on the analysis of lysergamides LSD, MIPLA, and LAMPA

Brandt

Kavanagh

Westphal³

et al. 2021

Drug Testing and Analysis

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Lysergic acid diethylamide (LSD) is a potent psychoactive substance that has attracted great interest in clinical research. As the pharmacological exploration of LSD analogs continues to grow, some of those analogs have appeared on the street market. Given that LSD analogs are uncontrolled in many jurisdictions, it is important that these analogs be differentiated from LSD. This report presents the analysis of blotters found to contain the N-methyl-N-isopropyl isomer of LSD (MIPLA), and techniques to differentiate it from LSD and the N-methyl-N-propyl isomer (LAMPA) under routine conditions. Gas chromatography (GC)-solid phase infrared spectroscopy was particularly helpful. GC-electron ionization-tandem mass spectrometry of the m/z 72 iminium ion also provided sufficient information to distinguish the three isomers on mass spectral grounds alone, where chromatographic separation proved challenging. Derivatization with 2,2,2-trifluoro-N,N-bis (trimethylsilyl)acetamide (BSTFA) also led to improved GC separation. Liquid chromatography single quadrupole mass spectrometry (LC-Q-MS) and in-source collision-induced dissociation allowed for the differentiation between MIPLA and LAMPA based on distinct m/z 239 ion ratios when co-eluting. An alternative LC-MS/MS method improved the separation between all three lysergamides, but LSD was found to co-elute with iso-LSD. However, a comparison of ion ratios recorded for transitions at m/z 324.2 > 223.2 and m/z 324.2 > 208.2 facilitated their differentiation. The analysis of two blotters by LC-Q-MS revealed the presence of 180 and 186 μg MIPLA per blotter. These procedures may be used to avoid inadvertent misidentification of MIPLA or LAMPA as LSD.

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Section: Resultsmentioning

confidence: 99%

Section: Lc-msmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 2 more Smart Citations

Separating the wheat from the chaff: Observations on the analysis of lysergamides LSD, MIPLA, and LAMPA

Brandt

Kavanagh

Westphal³

et al. 2021

Drug Testing and Analysis

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show abstract

“…An extensive interference study was conducted (104 compounds), and validation (see also Table 3) showed that the method displayed good linearity between 0.5 and 10 ng/mL (ensuring correct m/z 223 and 281 relative intensities to m/z 324 within a 10% error margin). In a second publication of the same group (White et al, 1997), identical LC±MS results were reported, without the immunoaf®nity extraction.…”

Section: Lsdmentioning

confidence: 71%

Liquid chromatography?mass spectrometry in forensic toxicology

Bocxlaer¹,

Clauwaert²,

Lambert³

et al. 2000

Mass Spectrom. Rev.

115

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Liquid chromatography—mass spectrometry has evolved from a topic of mainly research interest into a routinely usable tool in various application fields. With the advent of new ionization approaches, especially atmospheric pressure, the technique has established itself firmly in many areas of research. Although many applications prove that LC—MS is a valuable complementary analytical tool to GC—MS and has the potential to largely extend the application field of mass spectrometry to hitherto “MS‐phobic” molecules, we must recognize that the use of LC—MS in forensic toxicology remains relatively rare. This rarity is all the more surprising because forensic toxicologists find themselves often confronted with the daunting task of actually searching for evidence materials on a scientific basis without any indication of the direction in which to search. Through the years, mass spectrometry, mainly in the GC—MS form, has gained a leading role in the way such quandaries are tackled. The advent of robust, bioanalytically compatible combinations of liquid chromatographic separation with mass spectrometric detection really opens new perspectives in terms of mass spectrometric identification of difficult molecules (e.g., polar metabolites) or biopolymers with toxicological relevance, high throughput, and versatility. Of course, analytical toxicologists are generally mass spectrometry users rather than mass spectrometrists, and this difference certainly explains the slow start of LC—MS in this field. Nevertheless, some valuable applications have been published, and it seems that the introduction of the more universal atmospheric pressure ionization interfaces really has boosted interests. This review presents an overview of what has been realized in forensic toxicological LC—MS. After a short introduction into LC—MS interfacing operational characteristics (or limitations), it covers applications that range from illicit drugs to often abused prescription medicines and some natural poisons. As such, we hope it can act as an appetizer to those involved in forensic toxicology but still hesitating to invest in LC—MS. © 2000 John Wiley & Sons, Inc., Mass Spec Rev 19: 165–214, 2000

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Labetalol Hydrochloride

2010

Analytical Methods for Therapeutic Drug Monitoring and Toxicology

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Determination of lysergide in urine by high-performance liquid chromatography combined with electrospray ionisation mass spectrometry

Cited by 25 publications

References 16 publications

Separating the wheat from the chaff: Observations on the analysis of lysergamides LSD, MIPLA, and LAMPA

Separating the wheat from the chaff: Observations on the analysis of lysergamides LSD, MIPLA, and LAMPA

Liquid chromatography?mass spectrometry in forensic toxicology

Labetalol Hydrochloride

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