Abstract:
:A variety of hallucinogens of the lysergamide type has emerged on the drug market in recent years and one such uncontrolled derivative of lysergic acid diethylamide (LSD) is 1-propionyl-LSD (1P-LSD). Due to the high potency of LSD and some of its derivatives (common doses: 50-200 μg), sensitive methods are required for the analysis of biological samples such as serum and urine. The occurrence of an intoxication case required the development of a fully validated, highly sensitive method for the quantification of 1P-LSD and LSD in urine and serum using LC-MS/MS. Given that LSD is unstable in biological samples when exposed to light or elevated temperatures, we also conducted stability tests for 1P-LSD in urine and serum under different storage conditions. The validation results revealed that the analysis method was accurate and precise with good linearity over a wide calibration range (0.015-0.4 ng mL-1). The limit of detection (LOD) and the lower limit of quantification (LLOQ) of 1P-LSD and LSD in serum and urine were 0.005 ng mL-1 and 0.015 ng mL-1, respectively. The stability tests showed no major degradation of 1P-LSD in urine and serum stored at -20 °C, 5 °C or at room temperature for up to five days, regardless of protection from light. However, LSD was detected in all samples stored at room temperature showing a temperature-dependent hydrolysis of 1P-LSD to LSD to some extent (up to 21% in serum). Serum samples were particularly prone to hydrolysis possibly due to enzymatically catalyzed reactions. The addition of sodium fluoride prevented the enzymatic formation of LSD. The method was applied to samples obtained from the intoxication case involving 1P-LSD. The analysis uncovered 0.51 ng mL-1 LSD in urine and 3.4 ng mL-1 LSD in serum, whereas 1P-LSD remained undetected. So far pharmacokinetic data of 1P-LSD is missing, but with respect to the results of our stability tests and the investigated case rapid hydrolysis to LSD in-vivo seems more likely than instabilities of 1P-LSD in urine and serum samples.
journal_name
J Pharm Biomed Analjournal_title
Journal of pharmaceutical and biomedical analysisauthors
Grumann C,Henkel K,Stratford A,Hermanns-Clausen M,Passie T,Brandt SD,Auwärter Vdoi
10.1016/j.jpba.2019.05.062subject
Has Abstractpub_date
2019-09-10 00:00:00pages
270-276eissn
0731-7085issn
1873-264Xpii
S0731-7085(19)30013-5journal_volume
174pub_type
杂志文章abstract::A simple and sensitive high-performance liquid chromatographic method for the determination of piperacillin in plasma is described. A C8 reversed-phase column was used with a mobile phase consisting of methanol-water-triethylamine (550:450:4, v/v/v) adjusted to pH = 3 with orthophosphoric acid and UV detection at 270 ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(91)80142-v
更新日期:1991-01-01 00:00:00
abstract::A first-derivative spectrophotometric method for the determination of irbesartan (IRB) alone and in the presence of hydrochlorothiazide (HCT) is described. Measurements are made at the zero-crossing wavelength at 263.0 nm for IRB. The calibration graph was linear over the range 1.0-12.0 mg l(-1) of IRB, detection limi...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(02)00073-0
更新日期:2002-06-20 00:00:00
abstract::A robust gradient high performance liquid chromatographic (HPLC) procedure is described for the simultaneous determination of melphalan content and related impurities in melphalan drug substance. The sample solution is prepared in methanol and injected. A linear gradient from 5 to 60% acetonitrile in water containing ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(99)00011-4
更新日期:1999-07-01 00:00:00
abstract::A reversed-phase gradient elution system with methanol-triethylammonium phosphate buffer (83.3 mM, pH 6.0) as eluent on C(18)-bonded silica is described for the separation of 38 ribonucleotides, deoxynucleotides, cyclic nucleotides and deoxycyclic nucleotides in less than 33 min. The retention of the nucleotides can b...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(86)80046-2
更新日期:1986-01-01 00:00:00
abstract::This paper deals with the chiral separation of optical isomers of beta-methyl-amino acids by CE and HPLC using the principle of ligand-exchange. Capillary zone electrophoresis was carried out using Cu(II) complexes of L-4-hydroxyproline (L-4-Hypro), N-(2-hydroxypropyl)-L-4-hydroxyproline (HP-L-4-Hypro) and N-(2-hydrox...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(01)00616-1
更新日期:2002-01-15 00:00:00
abstract::4-Nitrobenzaldehyde is the synthetic raw material and an important photodegradation product of chloramphenicol. With a structural "alert" of human genotoxic potential and reported mutagenicity, this compound should be controlled in drug substances as a potential genotoxic impurity. However, current analysis methods re...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.04.024
更新日期:2018-07-15 00:00:00
abstract::The aim of the current study was to develop and validate a robust multi-analyte high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) method for simultaneous quantification of cefepime, meropenem, ciprofloxacin, moxifloxacin, linezolid and piperacillin, which are the most commonly used antibioti...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.01.031
更新日期:2018-04-15 00:00:00
abstract::S-Adenosyl-L-methionine (SAM) and its metabolites S-adenosyl-L-homocysteine (SAH) and methyl-thioadenosine (MTA) are endogenous compounds that are heavily involved in a variety of biochemical processes, and have therefore been the target for several assays in body fluids and tissues. Reversed-phase chromatographic beh...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(93)80029-z
更新日期:1993-04-01 00:00:00
abstract::Two cellulose-based chiral stationary phases (Chiralcel OD and Chiralcel OJ) were compared on their ability to resolve various aliphatic ibuprofen esters. Chiralcel OJ with hexane as the mobile phase allows for the separation of most of the esters. Observed changes in resolution depending on the solute nature (basicit...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(97)00212-4
更新日期:1998-03-01 00:00:00
abstract::A previously described isocratic liquid chromatographic (LC) method for the analysis of tetracycline on poly(styrene-divinylbenzene) allows the complete separation and resolution of tetracycline (TC), 4-epitetracycline (ETC), anhydrotetracycline (ATC) and 4-epianhydrotetracycline (EATC). By means of a half-fraction fa...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(93)80110-m
更新日期:1993-11-01 00:00:00
abstract::An UPLC-MS/MS method for the quantification of indirubin in lithium heparinized rat plasma was developed and validated according to current international guidelines. Indirubin was extracted from rat plasma by using Waters Ostro™ pass-through sample preparation plates. The method was validated with a LLOQ of 5.00ng/mL ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2016.05.018
更新日期:2016-09-05 00:00:00
abstract::A liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) assay was developed and qualified for analyzing 4β-hydroxycholesterol and cholesterol in 5 μl of human and mouse plasma. Stable isotope-labeled d7-analogs of both analytes were used as internal standards and 4.2% (w/v) human serum ...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2013.07.016
更新日期:2013-11-01 00:00:00
abstract::A selective and sensitive liquid chromatography-mass spectrometry (LC-MS) method was developed for the simultaneous determination of Euphorbia factor L(1), Euphorbia factor L(2) and Euphorbia factor L(3) from Euphorbiae semen in rat plasma. Larotaxel was added to a 200 μL plasma sample as the internal standard (IS). T...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2012.09.005
更新日期:2013-01-01 00:00:00
abstract::Maytenus ilicifolia is an important plant in Brazilian folk medicine, used in many gastric disorder treatments. Low molecular weight components present in the leaves have been characterized as afzelechin, epiafzelechin, catechin, epicatechin, gallocatechin and epigallocatechin, as detected by HPLC and ESI-MS. Condense...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2007.12.008
更新日期:2008-05-12 00:00:00
abstract::Ionic liquid dispersive liquid-liquid microextraction (IL-DLLME) was used for the first time for the extraction and preconcentration of cortisone and cortisol from human saliva samples. This approach allows the determination of both compounds by liquid chromatography (LC) with ultra-violet/visible (UV/Vis) detection a...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.12.001
更新日期:2019-02-20 00:00:00
abstract::Astragali Radix (AR) has been used in the traditional Chinese medicine (TCM) in the treatment of various renal diseases for many years. In this study, a NMR based metabolomic approach coupled with biochemical assay and histopathological inspection had been employed to study the protective effect of total flavonoids (T...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2018.05.045
更新日期:2018-09-05 00:00:00
abstract::A simple, rapid and sensitive method termed as dispersive liquid-liquid microextraction (DLLME) combined with high-performance liquid chromatography-ultraviolet detector (HPLC-UV) has been proposed for the determination of three psychotropic drugs (amitryptiline, clomipramine and thioridazine) in urine samples. The de...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2008.11.036
更新日期:2009-02-20 00:00:00
abstract::Human polyvalent intravenous immunoglobulin (IVIG) preparations are used as a complementary aid to the proper antimicrobial treatment of severely septic patients in intensive care units (ICUs) and/or as a prophylactic agent to immunocompromised hosts, particularly prone to bacterial infections. There is skepticism abo...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(99)00087-4
更新日期:1999-09-01 00:00:00
abstract::The present study deals with the stress degradation studies on amorphous and polymorphic forms of clopidogrel bisulphate. The objective was to characterize the degradation products and postulate mechanism of decomposition of the drug under solid state stress conditions. For that, amorphous form, polymorph I and polymo...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2009.05.001
更新日期:2010-07-08 00:00:00
abstract::A simple, rapid, reproducible and stability indicating high performance thin-layer chromatographic method for the analysis of Nimesulide both the bulk drug and from pharmaceutical formulations is reported. The mobile phase selected consists of Cyclohexane-Ethylacetate [60:40, v/v]. It gave compact spots both for Nimes...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(00)00597-5
更新日期:2001-06-01 00:00:00
abstract::A simple analytical method for l-menthol by high-performance liquid chromatography with a polarized photometric detector was established. The polarized photometric detector was constructed with two polarizers mounted on both sides of the flow cell in a conventional photometric detector and can be easily used for the d...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/s0731-7085(97)00146-5
更新日期:1998-04-01 00:00:00
abstract::It is shown that activity in the area of chemically modified electrodes continues at a high level. This topic is increasing in popularity with a large research field on the incorporation of electroactive groups into a variety of conductive films. These developments are also directed towards catalyzing bioselective and...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/0731-7085(86)80089-9
更新日期:1986-01-01 00:00:00
abstract::Platinum compounds, including cis-dichlorodiaminoplatinum(II) or cisplatin, are an important class of anti-cancer drugs, which should be carefully monitored in the biological fluids. In this study, electrodeposition coupled with electrothermal atomic absorption spectrometry (ETAAS) was used for determination of Pt con...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2010.02.023
更新日期:2010-09-21 00:00:00
abstract::A rapid and efficient chiral supercritical fluid chromatography (SFC) method has been developed for the quantitative determination of panthenol enantiomers in cosmetic formulations (cream, lotion, wipe, and exfoliant). Indeed, the pharmacological effect only depends on the D form (Dexpanthenol) thus accurate measureme...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2014.09.036
更新日期:2015-01-01 00:00:00
abstract::This review paper discusses the success of columns packed with superficially porous particles (SPP) in liquid chromatography for the analysis of peptides and proteins. First, it summarizes the history of SPP, including the development of different SPP generations from particles of 50 μm to sub-2 μm. It also critically...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章,评审
doi:10.1016/j.jpba.2018.06.006
更新日期:2018-09-05 00:00:00
abstract::The N-terminal glutamic acid (Glu) can be cyclized to form pyroglutamate (pGlu). Recent studies have suggested that N-terminal pGlu formation is an important posttranslational or co-translational event and is greatly facilitated by the enzyme glutaminyl cyclase, although the impact of the N-terminal cyclization on the...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2006.05.008
更新日期:2006-10-11 00:00:00
abstract::A novel strategy for predicting bioactive components in traditional Chinese medicines (TCM) using live cell extraction and high performance liquid chromatography-diode array detection-mass spectrometry (HPLC-DAD-MS) analysis was proposed. The hypothesis is that when cells are incubated together with the extract of TCM...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2006.01.014
更新日期:2006-05-03 00:00:00
abstract::Polyoxypregnane and its glycosides (POPs) are frequently present in plants of Asclepiadaceae family, and have a variety of biological activities. There is a great need to comprehensively profile these phytochemicals and to quantify them for monitoring their contents in the herbs and the biological samples. However, PO...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2017.06.038
更新日期:2017-10-25 00:00:00
abstract::A health supplement used for sexual performance enhancement was sent to Health Sciences Authority of Singapore for testing. An unknown compound was detected and isolated and its structure was elucidated using NMR, high-resolution MS, ESI-MS/MS, UV and IR. The compound, dapoxetine, is reported to be a selective seroton...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2009.06.005
更新日期:2009-12-05 00:00:00
abstract::A new agar-free bioautographic assay for xanthine oxidase (XO) inhibitors and superoxide scavengers on TLC layers was developed and validated. Compared to the first version of TLC bioautographic agar overlay method, our bioautographic assay greatly improved the sensitivity and quantification ability. The limit of dete...
journal_title:Journal of pharmaceutical and biomedical analysis
pub_type: 杂志文章
doi:10.1016/j.jpba.2017.11.077
更新日期:2018-02-20 00:00:00