Instrumental Data for Drug Analysis

Mills, Terence C.; Roberson, J. Conrad; Wall, William H.; Lothridge, Kevin L.; McDougall, William D.; Gilbert, Michael W.

doi:10.4324/9781351073714

Cited by 2 publications

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“…A partial section (650-1900 cm À1 ) of the GC-sIR spectra recorded for LSD, MIPLA, and LAMPA is shown in Figure 8 to allow for a spectral comparison (full spectra and overlaid spectra are supplied as Supporting Information). The spectrum of LSD was consistent with others reported in the literature (e.g., Mills et al 27 ) including signals typical for other lysergamides at 1627 (C=O str ), 1448 (C-N str ), and 779 and 749 cm À1 that might have been associated with C-H out of plane deformation vibrations in the indole part of the molecule. 67 A visual inspection of all three spectra in Figure 8 revealed distinct differences.…”

Section: Spectroscopic Featuressupporting

confidence: 90%

“…It is recommended to consider increasing the scan range to capture this ion. Recorded (or displayed) scan ranges reported for LAMPA spectra previously included m/z 150-350, 7 m/z 50-330, 19 m/z 50-330, 20 m/z 40-340, 8 m/z 25-400, 22 m/z 40-360, 15 m/z 20-336,, 24 m/z 40-330, 27 and m/z 29-600. 25 As suggested previously by other authors, inclusion of lower masses into the scan range requires particular attention to cleanliness of the instrumentation to minimize appearance of low mass impurities.…”

Section: Gc-msmentioning

confidence: 99%

“…IR spectra of LSD 7,11,15,21,24,26,27,[63][64][65][66][67][68][69] and LAMPA 7,11,15,21,24,26,27 have been published previously. The extent to which a direct comparison between spectral data collected from lysergamide samples can be made depends on various factors such as the presence of salt or base forms (or mixtures), how the sample was prepared for the IR measurement, and how the data were recorded.…”

Section: Spectroscopic Featuresmentioning

confidence: 99%

“…These involved high-performance liquid chromatography (HPLC), 8,[10][11][12][13][14][15][16][17] gas chromatography (GC), 8,[14][15][16][18][19][20][21][22][23][24][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][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.…”

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: Spectroscopic Featuressupporting

confidence: 90%

Section: Gc-msmentioning

confidence: 99%

Section: Spectroscopic Featuresmentioning

confidence: 99%

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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“…The brands used (A: Innovator product, B: Generic product-Indian origin, and C: Generic product Indian origin) [7][8][9][10].…”

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2018

LOJMS

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Cephalosporins are the highly used Broad-spectrum antibiotics, belong to β-lactam class. Cephalosporins resemble penicillin in that they have a β-lactam structure, but the five-member thiazolidine ring characteristic of the penicillin is replaced by a sixmember dihydrothiazine ring. The bactericidal action of beta lactam antibiotics is directly attributable to their ability to react with PBP's. The research work relates to a by-products during process for the industrial manufacture of Cefpodoxime Proxetil. The drug is registered in USP and belongs to 3rd generation drug. It was discovered by Brotzu in fungus Cephalosporium Acremonium which produces a chemical which show antimicrobial activity. Abraham isolated the three fragmentation patterns of cefpodoxime proxetil. Data from this systematic study will help improve the safety and quality of cefpodoxime proxetil types of cephalosporin antibiotics cephalosporin P, cephalosporin N, cephalosporin C.7-ACA is widely used as the substrate for synthesizing cephalosporin antibiotics. Modification of the 7-ACA side-chains resulted in the development of useful antibiotic agents, and the first agent is Cephalothin (cefalotin) was launched by. Eli Lilly Company in 1964 There are many patents which gives the procedure of Synthesis of Cefpodoxime ProxetilStability of three Cefpodoxime proxetil products available in indian market at fridge temperatures (2-8 °C), room temperature (25 °C) and elevated temperature (42 °C). Flow properties, rheological and the physicochemical parameters of both powder and reconstituted powder were used to evaluate the stability of different brands of Cefpodoxime proxetil available in india. The powder of stability samples was eluted through a C18 column with formic acid-methanol-water as the mobile phase. In total, 15 impurities were characterized in commercial samples, including 7 known impurities and 8 new impurities. The structures of these unknown compounds were deduced via comparison.

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Instrumental Data for Drug Analysis

Cited by 2 publications

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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

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