Simultaneous Determination of 17 Toxic Alkaloids in Human Fluids by Liquid Chromatography Coupled With Electrospray Ionization Tandem Mass Spectrometry

Abstract

A sensitive and specific method was proposed and validated for the simultaneous determination of 17 poisonous alkaloids in human blood and gastric juice by liquid chromatography and electrospray ionization tandem mass spectrometry (LC-ESI-MS=MS). After mixing with boric acid buffer solution (pH 9), the samples were extracted with chloroform followed by chloroform-ether (2:1, v=v). The simultaneous qualitative and quantitative analysis of 17 alkaloids, including koumine, atropine, scopolamine, brucine, strychnine, aconitine, bulleyaconitine A, ephedrine, pilocarpine, lobeline, ergometrine, anabasine, oxymatrine, theophylline, colchicine, tetrahydropalmatine, and eserine, were performed by using ESI þ in multiple-reaction monitoring (MRM) mode. Under the optimized conditions, the calibration curves of the 17 compounds presented good linearity (r=0.9952) in the ranges of 0.5-50 lg=L and 0.5-500 lg=L. The quantitation limits (LOQs) and detection limits (LODs) ranged from 0.5-1 and 0.1-0.5 lg=L, respectively. The average extraction recoveries were obtained in the range of 81.7-102.3 %. The intra-day and inter-day relative standard deviations (RSDs) were less than 10% and 15 %, respectively. The results indicated that the method was simple, rapid, selective, sensitive, and stable enough to examine toxic alkaloids and was suitable for poisoning diagnosis and forensic toxicology.

Sample Preparation and Bioanalysis Validation for Natural Product Sample

“…The four types of flavonoids are schaftoside, isovitexin, luteolin, and apigenin as well as one phenolic acid which is ferulic acid in the biological matrix of rat plasma and sulfamethoxazole is used as an internal standard (IS) [17]. Another natural product, Glycyrrhiza, which is a popular drug in China that has been used for years as an anti-cancer, anti-ulcer, anti-inflammatory, antiviral, and for improving liver function [19]. ).…”

“…This herbal remedy is used as a treatment for kidney stones. The extraction sample preparation used was the protein deposition method [17,19]. A methanol solvent was used to extract four flavonoids and phenolic acids from the extract of Herba Desmodii Styracifolii in plasma.…”

“…Validation of the bioanalysis method includes all procedures which show that the specific method used for quantitative measurement of analyte originating in the biological matrix. The basic parameters of validation aim to determine quality which includes criteria such as selectivity, sensitivity, linearity, accuracy, precision, stability, quantification limit (LOQ), recovery (recovery), limit of detection (LOD), reproductivity and roughness [10][11][12][13][14][15][16][17][18][19][20][21]. Therefore, this paper aims to discuss various types of sample preparation techniques and bioanalysis validation for natural products, which include information on various biological sample collection and preparation techniques, discussion of biological sample preparation techniques, and discussion of the application of bioanalysis to various products natural compound.…”

Determination of ephedrine, pseudoephedrine, sinapine thiocyanate, tetrahydropalmatine and amygdalin by HPLC-MS/MS after oral administration of extracts of Majie cataplasm in rabbits plasma: Application to a pharmacokinetic study

“…In the previous studies, several detection methods have been developed, including LC-MS/MS method for E, PE and AG in rats (Jiang et al, 2015), LC-MS/MS method for ST and THP in plasma , LC-ESI-MS/MS method for E and THP in human blood (Wu et al, 2013). However, to our best knowledge, these methods had limitation such as high limit of detection, which was not adequate to meet current needs.…”

Simultaneous determination of eight alkaloids and oleandrin in herbal cosmetics by dispersive solid‐phase extraction coupled with ultra high performance liquid chromatography and tandem mass spectrometry

“…By utilizing micro LLE and GC–MS/MS, Zhu determined the residuals of five poisonous alkaloids (hyoscyamine, scopolamine, gelsemine, strychnine, and brucine) in food . What is more, Lin established a HPLC–MS/MS method to simultaneously determine 17 kinds of alkaloids in blood and gastric juice . However, the above determination methods of alkaloids mainly focus on medicine, blood or serum, which are quite different from herbal cosmetics.…”