气相色谱/质谱检验合成大麻素K3中AKB48

目的建立较为快速准确的合成大麻素K3中AKB48的气相色谱/质谱检验方法。方法对进样口温度、初始柱温、柱流速及质谱采样率等4项色谱及质谱实验参数进行考察优化。结果 GC/MS检验合成大麻素K3中AKB48的优化条件为:进样口温度280℃,柱初始温度80℃,柱流速为2.0ml/min,质谱采样率为2。结论该方法具有快速、准确、灵敏等优点,可用于K3中AKB48的定性检验鉴定。     

GC／MS同时分析头发中大麻酚类和△^9-四氢大麻酸

目的建立同时分析毛发中THC、CBN、CBD和大麻主要代谢物THC-COOH的方法.方法头发检材去污处理后,加入内标氯灭酸,经NaOH水解和正己烷:乙酸乙酯(9:1)提取,吹干后衍生化,利用GC/MS-SIM方法分析.结果THC、CBN和THC-COOH的最低检出限分别为0.01、0.05和0.01ng/mg.10例阳性头发中均检出THC成分,THC浓度范围为0J 1～8.84ng/mg,有3例未检出THC-COOH,检出者的量亦低于定量下限.结论同时分析头发中的大麻酚类和△9-四氢大麻酚是可行的,头发中THC-COOH浓度明显都低于THC浓度.     

Rapid Identification of Synthetic Cannabinoids in Herbal Incenses with DART‐MS and NMR

The usage of herbal incenses containing synthetic cannabinoids has caused an increase in medical incidents and triggered legislations to ban these products throughout the world. Law enforcement agencies are experiencing sample backlogs due to the variety of the products and the addition of new and still‐legal compounds. In our study, proton nuclear magnetic resonance (NMR) spectroscopy was employed to promptly screen the synthetic cannabinoids after their rapid, direct detection on the herbs and in the powders by direct analysis in real time mass spectrometry (DART‐MS). A simple sample preparation protocol was employed on 50 mg of herbal sample matrices for quick NMR detection. Ten synthetic cannabinoids were discovered in fifteen herbal incenses. The combined DART‐MS and NMR methods can be used to quickly screen synthetic cannabinoids in powder and herbal samples, serving as a complementary approach to conventional GC‐MS or LC‐MS methods.     

Identification of Eight Synthetic Cannabinoids,Including 5F‐AKB48 in Seized Herbal Products Using DART‐TOF‐MS and LC‐QTOF‐MS as Nontargeted Screening Methods

Synthetic cannabinoids are sprayed onto plant material and smoked for their marijuana‐like effects. Clandestine manufacturers modify synthetic cannabinoid structures by creating closely related analogs. Forensic laboratories are tasked with detection of these analog compounds, but targeted analytical methods are often thwarted by the structural modifications. Here, direct analysis in real time coupled to accurate mass time‐of‐flight mass spectrometry (DART‐TOF‐MS) in combination with liquid chromatography quadruple time‐of‐flight mass spectrometry (LC‐QTOF‐MS) are presented as a screening and nontargeted confirmation method, respectively. Methanol extracts of herbal material were run using both methods. Spectral data from four different herbal products were evaluated by comparing fragmentation pattern, accurate mass and retention time to available reference standards. JWH‐018, JWH‐019, AM2201, JWH‐122, 5F‐AKB48, AKB48‐N‐(4‐pentenyl) analog, UR144, and XLR11 were identified in the products. Results demonstrate that DART‐TOF‐MS affords a useful approach for rapid screening of herbal products for the presence and identification of synthetic cannabinoids.     

Quantitative Determination of Cannabinoids in Cannabis and Cannabis Products Using Ultra‐High‐Performance Supercritical Fluid Chromatography and Diode Array/Mass Spectrometric Detection

Ultra‐high‐performance supercritical fluid chromatography (UHPSFC ) is an efficient analytical technique and has not been fully employed for the analysis of cannabis. Here, a novel method was developed for the analysis of 30 cannabis plant extracts and preparations using UHPSFC /PDA ‐MS . Nine of the most abundant cannabinoids, viz . CBD , ?⁸‐THC , THCV , ?⁹‐THC , CBN , CBG , THCA ‐A, CBDA , and CBGA , were quantitatively determined (RSD s < 6.9%). Unlike GC methods, no derivatization or decarboxylation was required prior to UHPSFC analysis. The UHPSFC chromatographic separation of cannabinoids displayed an inverse elution order compared to UHPLC . Combining with PDA ‐MS , this orthogonality is valuable for discrimination of cannabinoids in complex matrices. The developed method was validated, and the quantification results were compared with a standard UHPLC method. The RSD s of these two methods were within ±13.0%. Finally, chemometric analysis including principal component analysis (PCA ) and partial least squares‐discriminant analysis (PLS ‐DA ) were used to differentiate between cannabis samples.     

Potency Trends of Δ9‐THC and Other Cannabinoids in Confiscated Cannabis Preparations from 1993 to 2008*

Abstract: The University of Mississippi has a contract with the National Institute on Drug Abuse (NIDA) to carry out a variety of research activities dealing with cannabis, including the Potency Monitoring (PM) program, which provides analytical potency data on cannabis preparations confiscated in the United States. This report provides data on 46,211 samples seized and analyzed by gas chromatography‐flame ionization detection (GC‐FID) during 1993–2008. The data showed an upward trend in the mean Δ⁹‐tetrahydrocannabinol (Δ⁹‐THC) content of all confiscated cannabis preparations, which increased from 3.4% in 1993 to 8.8% in 2008. Hashish potencies did not increase consistently during this period; however, the mean yearly potency varied from 2.5–9.2% (1993–2003) to 12.0–29.3% (2004–2008). Hash oil potencies also varied considerably during this period (16.8 ± 16.3%). The increase in cannabis preparation potency is mainly due to the increase in the potency of nondomestic versus domestic samples.     

固相微萃取技术在毛发药物分析中的应用

固相微萃取（SPME）可与GC/MS、HPLC/MS等在线联用,实现分离、分析一体化的特点为其在毛发药物分析中的应用提供了可能性和良好的应用前景。本文对SPME技术在毛发中滥用药物如苯丙胺类、美沙酮、大麻、可卡因、利多卡因等及其相应代谢产物的分析研究及应用进展做一综述。     

合成大麻素检验方法研究进展

近年合成大麻素类物质(synthetic cannabinoids,SCs)的危害及滥用引起社会广泛关注,它们不仅具有类似天然大麻的致幻性,还有更强的副作用,包括潜在的神经精神毒性,严重影响人类身心健康。因此,国内外研究人员对合成大麻素及其代谢物的检验方法进行了相关研究。本文主要介绍了SCs的生理药理作用、主要分类等,对其检验方法研究进展进行了综述与展望,探讨了各检验方法的应用范围与选择依据,以期为SCs相关案件的检验鉴定提供参考。     

Detection of Brodifacoum and other Rodenticides in Drug Mixtures using Thermal Desorption Direct Analysis in Real Time Mass Spectrometry (TD‐DART‐MS)

In recent months, there has been increased reporting of seized drug and toxicology cases containing rodenticides, the active ingredient in rat poisons. Seeing as rodenticides are not scheduled substances, they are not commonly screened for in seized drug analysis. This work investigates the use of TD‐DART‐MS for the simultaneous detection of rodenticides and drugs. Six rodenticides were evaluated, an optimal method was established, and limits of detection in the tens of nanograms were calculated. Additional studies highlight that detection at less than 1% by weight in mixtures with AB‐FUBINACA, cocaine, heroin, or methamphetamine was possible. This work presents an optimized method for detection of these compounds, allowing for the simultaneous detection of drugs and rodenticides, providing drug chemists with a tool for rapid identification of these compounds for forensic or public health purposes.