ABSTRACT
ABSTRACT: Objective To establish a method combining QuEChERS and ultra-high liquid chromatography-tandem mass spectrometry ï¼UPLC-MS/MSï¼ for rapid screening and testing of three types of new psychoactive tryptamines in human bloodï¼ 5-MeO-DALT, 5-MeO-MiPT and 5-MeO-DiPT. Methods The effects of the type of extractant, the type and dosage of salting-out agent, and the dosage of adsorbent on the test results of the three tryptamines were investigated. Blood samples were processed by QuEChERS method and then determined by UPLC-MS/MS. Results The linear relationships of 5-MeO-DALT, 5-MeO-MiPT and 5-MeO-DiPT in human blood were good in the range of 0.5-100, 0.5-100 and 0.2-100 ng/mL, respectively, with their coefficients higher than 0.99. The limits of detection ï¼LODsï¼ were 0.1-0.2 ng/mg. The recoveries ranged from 84.86% to 94.57%. Intra-day and inter-day precisions were good. Conclusion The method is simple, rapid, easy to operate and has a high recovery. It is suitable for the qualitative and quantitative study of tryptamines in blood and can provide the reference for public security organs to deal with related cases.
Subject(s)
Tandem Mass Spectrometry , Tryptamines , Chromatography, High Pressure Liquid , Chromatography, Liquid , Humans , Limit of DetectionABSTRACT
ABSTRACT: Objective To investigate the maximum allowable deviations of retention time and ion abundance ratio of the 8 common drugs ï¼poisonsï¼ from 3 categories, poisons ï¼methamphetamine, morphine, ketamineï¼, benzodiazepines ï¼estazolam, midazolam, diazepam, clonazepamï¼ and barbiturates ï¼phenobarbitalï¼ in blood, by liquid chromatography-tandem mass spectrometry ï¼LC-MS/MSï¼ in forensic toxicology analysis. Methods The deviations of retention time and ion abundance ratio at 7 low mass concentrations, limit of detection ï¼LODï¼, 2LOD, limit of quantitation ï¼LOQï¼, 1.5LOQ, 2LOQ, 4LOQ and 6LOQ, were tested by LC-MS/MS after liquid-liquid extraction under the conditions of two chromatographic columns and three chromatographs. Results The deviation of absolute retention time of 98.11% of 8 drugs ï¼poisonsï¼ in the blood samples was within the range of ±0.05 min, and that of the relative retention time of 96.21% was within the range of ±0.4%. The maximum deviation of the ion abundance ratio was highly correlated with the mass concentration. When the mass concentration of drugs ï¼poisonsï¼ was LOQ or above, more than 95% of the absolute deviation and relative deviation of the ion abundance ratio were in the range of ±25% and ±40%, respectively; when the mass concentration was below LOQ, the range could be expanded to ±35% and ±50%, respectively. Conclusion It is recommended for the determination range of the absolute retention time deviation of 8 common drugs ï¼poisonsï¼ to be ±0.1 min and that of the relative retention time deviation to be ±1.0%. The determination range of absolute deviation of the ion abundance ratio should be ±25% when the mass concentration is LOQ or above, and the relative deviation should be ±40%. When the mass concentration is below LOQ, the deviation determination range can be expanded to ±35% and ±50%, respectively.
Subject(s)
Tandem Mass Spectrometry , Chromatography, Liquid , Forensic Toxicology , Liquid-Liquid Extraction , PoisonsABSTRACT
ABSTRACT: Objective To investigate the maximum allowable deviation of ion abundance ratios of characteristic fragment ions in common drugs ï¼poisonsï¼ in blood by gas chromatography-mass spectrometry ï¼GC-MSï¼ method. Methods Four common drugs ï¼poisonsï¼ ï¼dichlorvos, phorate, diazepam and estazolamï¼ were detected by GC-MS full scan mode after liquid-liquid extraction in two laboratories and under three chromatographic conditions. The deviations of ion abundance ratios of the four common drugs ï¼poisonsï¼ in marked blood samples with concentrations of 0.5, 1.0, 2.0, 5.0 and 10.0 µg/mL were analyzed. At the same time, the false negative rates of ion abundance ratios were analyzed when the mass concentration was limit of detection ï¼LODï¼, 2LOD, limit of quantitation ï¼LOQï¼ and 2LOQ, and the false positive rates of ion abundance ratios were analyzed with blank blood samples. Results Under the two laboratories, four common drugs ï¼poisonsï¼ and three kinds of chromatography conditions, the differences in deviations of the ion abundance ratios of marked blood samples were not statistically significant ï¼P>0.05ï¼. More than 95% of the absolute deviations of the ion abundance ratios of the marked blood samples were within the range of ±10%, and more than 95% of the relative deviations were within the range of ±25%. In cases of low concentration ï¼concentration less than 2LOQï¼ or low signal to noise ratio ï¼3-15ï¼, the false negative rate was less than 5% and the false positive rate was 0% when the relative deviation was greater than 50%. Conclusion The absolute deviations of ion abundance ratios of four common drugs ï¼poisonsï¼ in marked blood samples are advised to have a determination range within ±10%, and the determination range of relative deviations within ±25%.
