Forensic Toxicology
·
2018
·Vol. 37
·期 1
·121-131
·
IF 3.924
Chen Lizhu,Yu Yingjia,Wang Yang,Xiang Ping,Duan Gengli
Purpose It is crucial for forensic analysis to differentiate clinical use from illegal abuse. Selegiline (SG) is mainly metabolized to desmethylselegiline (DM-SG), R -(−)-methamphetamine (R-MA) and R-(−)amphetamine (R-AM); while abused methamphetamine and amphetamine mainly contain the S -(+)-form. The aim of this study was to simultaneously determine SG, DM-SG, R / S -MA, and R / S -AM in human oral fluid (OF) and to differentiate clinical use from illegal use. We also aim to apply the present method to the OF samples from authentic cases in forensic toxicology. Methods Liquid–liquid extraction and liquid chromatography-tandem mass spectrometry operating in positive ion multiple-reaction monitoring mode were utilized. The chromatographic system consisted of a Chirobiotic TM V2 column (2.1 mm × 250 mm, 5 μm) and a mobile phase of methanol containing 0.1% (v/v) glacial acetic acid and 0.02% (v/v) ammonium hydroxide. Results and conclusions The calibration curves were linear from 1 to 100 ng/mL, and r > 0.995 for all analytes with imprecisions ≤ 15% and accuracy between 85 and 115%. Extraction recoveries ranged from 46.3 to 104.7% with coefficient of variation (CV) ≤ 10.3% and matrix effects (MEs) ranged from 47.4 to 114.8% with CV ≤ 12.9%. The lower limit of quantification was 0.2 ng/mL for SG and DM-SG and 1.0 ng/mL for S-MA, R-MA, S-AM and R-AM. The present method is simple, rapid (accomplished in 12 min), sensitive, and validated by authentic samples.
研究领域:
法医学
·
分析化学
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产品关联
DOI
高影响因子
Frontiers in Chemistry
·
2019
·
IF 3.782
Chen Lizhu,Yu Yingjia,Duan Gengli,Wang Xin,Shen Baohua,Xiang Ping
Objective: Chiral analysis is a crucial method to differentiate selegiline intake from drug abuse. A dried urine spot (DUS) analytical method based on spotting urine samples (10 μL) onto dried spot collection cards, and followed by air-drying and extraction, was developed and validated for the determination of selegiline, desmethylselegiline, R/S-methamphetamine, and R/S-amphetamine.Methods: Methanol (0.5 mL) was found to be the ideal extraction solvent for target extraction from DUSs under orbital-horizontal stirring on a lateral shaker at 1,450 rpm for 30 min. Determinations were performed by direct electrospray ionization tandem mass spectrometry (ESI-MS/MS) under positive electrospray ionization conditions using multiple reaction monitoring mode. The chromatographic system consisted of a ChirobioticTM V2 column (2.1 × 250 mm, 5 μm) and a mobile phase of methanol containing 0.1% (v/v) glacial acetic acid and 0.02% (v/v) ammonium hydroxide.Results and conclusions: The calibration curves were linear from 50 to 5,000 ng/mL, with r > 0.995 for all analytes, imprecisions ≤ 15% and accuracies between −11.4 and 11.7%. Extraction recoveries ranged from 48.6 to 105.4% with coefficients of variation (CV) ≤ 13.7%, and matrix effects ranged from 45.4 to 104.1% with CV ≤ 10.3%. The lower limit of quantification was 50 ng/mL for each analyte. The present method is simple, rapid (accomplished in 12 min), sensitive, and validated by a pharmacokinetic study in human urine collected after a single oral administration of SG.
研究领域:
分析化学
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药理学
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毒理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2020
·
IF 3.004
Yanshuxian Liu,Yilei Fan,Zhongping Huang,Huijun Liu,Lili Wang,Zhenlu Shen,Ichi Watanabe
A rapid and sensitive method utilizing flash evaporation-gas chromatography/mass spectrometry (FE-GC/MS) has been developed. The method is applicable to determine ketamine (KET), methamphetamine (MAMP) and 3,4-methylenedioxymethamphetamine (MDMA) in human hair. Cut and weighted hair (0.30 mg) was heated at the flash evaporation temperature of 350 °C. KET, MAMP and MDMA were released into a capillary column for GC/MS analysis and produced fragment ions in SIM mode. Validation of the method included evaluation of linearity, sensitivity, accuracy, precision and repeatability. Linearity ranged from 2 to 300 ng/mg for KET in hair and 2 to 200 ng/mg for MAMP and MDMA in hair with the correlation coefficients all greater than 0.998. Limits of detection were 0.7 ng/mg and limits of quantification were 2.0 ng/mg of hair for KET, MAMP and MDMA. The precision ranged from 1.57% to 7.75% for KET, 1.49% to 7.10% for MAMP and 1.84% to 8.31% for MDMA. The recovery ranged from 102.1% to 110.9% for KET, 99.3% to 108.0% for MAMP and 89.5% to 112.6% for MDMA. Six authentic hair samples from known drug abusers and three drug-free hair samples from volunteers who had never used drugs were successfully analyzed. Compared with traditional time-consuming and hair-comsuming pretreatment method, FE-GC/MS was a faster, simpler and low sample consumption method for the determination of KET, MAMP and MDMA in human hair.
研究领域:
毒理学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MOLECULES
·
2022
·Vol. 27
·期 12
·3939
·
IF 4.927
Yazhou Qin,Fan Mo,Sen Yao,Yuanzhao Wu,Yingsheng He,Weixuan Yao
Porous noble metal nanomaterials have attracted extensive attention due to their high specific surface area and surface plasmon resonance effect. However, it is difficult to form porous structures due to the high mobility and low reduction potential of noble metal precursors. In this article, we developed a facile method for preparing porous Ag with a controllable structure at room temperature. Two kinds of Ag crystals with different porous structures were successfully prepared by using AgCl cubes as sacrificial templates. Through the galvanic replacement reaction of Zn and AgCl, Ag crystals with a sponge-like porous structure were successfully prepared. Additionally, using NaBH4as the reducing agent, we prepared granular porous Ag cubes by optimizing the amount of reducing agent. Both the sponge-like and granular porous Ag cubes have clean and accessible surfaces. In addition, we used the prepared two porous Ag cubes as substrate materials for SERS detection of five kinds of methamphetamine analogs. The experimental results show that the enhancement effect of granular porous Ag is better than that of sponge-like porous Ag. Furthermore, we probed the hot spot distribution of granular porous Ag by Raman mapping. By using granular porous Ag as the substrate material, we have achieved trace detection of 5 kinds of methamphetamine analogs including Ephedrine, Amphetamine, N-Methyl-1-(benzofuran-5-yl)propan-2-amine (5-MAPB), N-Methyl-1-(4-methoxyphenyl)propan-2-amine (PMMA) and N-Methyl-1-(4-fluorophenyl)propan-2-amine (4-FMA). Furthermore, to achieve qualitative differentiation of analogs with similar structures we performed density functional theoretical (DFT) calculations on the Raman spectra of the above analogs. The DFT calculations provided the vibrational frequencies, Raman activities, and normal mode assignment for each analog, enabling the qualitative differentiation of the above analogs.Keywords:Ag crystal;methamphetamine;SERS;porous structure
研究领域:
化学
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材料科学
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分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHEMICAL AND ENGINEERING DATA
·
2025
·
IF 2.1
Jingxuan Qiu,Rui Zhang,Chaoqun Zhang,Jing Lin,Cong Liu,Yunchun Guo,Huiliang Wang,Yingxin Xie,Ke Xiao
In this work, the solubility of phenprobamate in water, acetone, 2-butanone, methyl acetate, ethyl acetate, methanol, ethanol, n-propanol, isopropanol, n-butanol, sec-butanol, and 1-pentanol was determined by a static gravimetric method at temperatures ranging from 283.15 to 323.15 K under atmospheric pressure. The solubility magnitudes increase monotonously with the increase of temperature in each solvent. The solubility is roughly ranked as propanone > methyl ethyl ketone > acetic acid methyl ester > ethyl acetate > water in non-alcohol solvents and methanol > 1-pentanol > sec-butanol > ethanol > n-butanol > n-propanol > isopropanol in alcohols. The solubility of phenprobamate could be ultimately determined by the combined influence of solvent polarity, hydrogen bond acceptor propensities, solvent–solvent intermolecular interactions, and spatial steric hindrance. In addition, the solubility data were correlated by the Apelblat model and the Yaws model. The outcomes show that the two models could both satisfactorily fit the experimental data, in which the Yaws model is more appropriate to correlate the solubility of phenprobamate compared with the Apelblat model. The data reported in this work contribute to the further crystallization and separation process of phenprobamate.
研究领域:
化学工程
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药物化学
✓ 已验证
产品关联
DOI
高影响因子
SURFACE & COATINGS TECHNOLOGY
·
2023
·
IF 5.4
Liping Yan,Siming Yan,Yi He,Yi Fan,Xinyu Cheng,Huilian Zhou,Jiamin Zhong,Zhiyuan Li,Jinxue Song,Hongjie Li
In this study, propylamine and ethylenediamine intercalated α-ZrP nanocomposites (denoted by P-α-ZrP and E-α-ZrP, respectively) were synthesized. The effects of propylamine and ethylenediamine intercalated α-ZrP nanocomposites and their reinforcements on the corrosion resistance and mechanical properties of Ni-B coatings were investigated and compared. The morphology and structure of the three composites were characterized using transmission electron microscopy, atomic force microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, infrared spectroscopy, thermogravimetric analysis, and particle size analysis. Both propylamine and ethylenediamine intercalation increase the layer spacing of α-ZrP, but do not change the lamellar structure of α-ZrP. The EIS test results show that both Ni-B/P-α-ZrP and Ni-B/E-α-ZrP composite coatings have significantly lower corrosion rates than Ni-B and Ni-B/α-ZrP composite coatings. Compared to Ni-B/α-ZrP, the corrosion rates are reduced by 32 % and 76 % respectively. The R ct values for Ni-B/P-α-ZrP and Ni-B/E-α-ZrP composite coatings are also distinctly higher than Ni-B/α-ZrP, with Ni-B/E-α-ZrP having the highest values. In addition, Ni-B/P-α-ZrP and Ni-B/E-α-ZrP composite coatings are both harder than Ni-B/α-ZrP and have lower average coefficients of friction and wear rates than Ni-B/α-aZrP. Among them, the Ni-B/E-α-ZrP composite coating has the highest microhardness (1163.64 ± 21.20 HV) and the best wear resistance. The wear rate is reduced by 87 % and 65 % compared to Ni-B and Ni-B/α-ZrP composite coatings respectively. In conclusion, both P-α-ZrP and E-α-ZrP are better than α-ZrP in terms of enhancement, with E-α-ZrP being the best.
研究领域:
材料科学
·
电化学
·
表面工程
✓ 已验证
产品关联
DOI
高影响因子
FORENSIC SCIENCE INTERNATIONAL
·
2014
·
IF 2.115
Binling Zhu,Liang Meng,Kefang Zheng
Recently a new type of mixed drug oral solution has become prevalent in China, the identification and quantitative inspection of which are demanded in conviction and sentencing as well as drug intelligence. In 2013, inspection was carried out on 86 bottles of substances seized in 13 cases with the adoption of GC–MS methodology for qualitative identification and GC–FID for quantitative identification. 94.1% of the samples were light yellow turbid liquid while 95.3% were detected with more than two drugs. Detection rate of methamphetamine, MDMA and ketamine was up to 89.5%, 37.2% and 83.7% respectively. Quantitative inspection results indicated that concentrations of methamphetamine, MDMA , ketamine were 0.04–13 mg/mL, 0.04–29 mg/mL and 0.1–34 mg/mL, respectively. Appearance, composition and drug concentration of samples vary from case to case.
研究领域:
毒理学
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分析化学
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法医学
✓ 已验证
DOI
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2021
·Vol. 413
·期 16
·4237-4246
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IF 4.157
Liu Hui,Xia Lei,Shen Chengyin,Huang Chaoqun,Chu Yannan
Methamphetamine (MA) is a highly addictive and illegal psychostimulant drug and is currently one of the most commonly abused illicit drugs in the world. The on-site rapid detection of trace amounts of MA and screening illicit drugs in clandestine laboratories is important for drug enforcement agencies and the forensic community in general. However, detecting methamphetamine in the presence of nicotine and cigarette smoke by ion mobility spectrometry faces difficulty due to the overlapped spectral peaks of methamphetamine and nicotine. In this work, a new method was developed to detect MA using pyridine as a dopant in the presence of nicotine by a homemade ion mobility spectrometry. The reduced mobilities of MA and nicotine were measured under the temperatures of the drift tube from 40 to 120 °C and doping with pyridine. The result shows that the temperature of 100 °C is beneficial to resolve the two substances. The concentration of doped pyridine is optimized to be 18 ppm. In this doped experiment, the reaction rate of nicotine is higher than that of MA by measuring the instrumental responses of MA and nicotine. No matter how high the nicotine content is, the interference of nicotine can be eliminated in the detection of MA doped with pyridine. This method is also successfully applied for the determination of MA and nicotine simultaneously in real saliva samples. The limit of detection of MA was measured to be about 0.5 ng/μL. The promising results in this work provide an effective method for on-site detection of MA. Graphical abstract
研究领域:
分析化学
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法医学
·
药物检测
✓ 已验证
DOI
高影响因子
ANALYTICAL SCIENCES
·
2019
·Vol. 35
·期 8
·875-882
·
IF 1.618
Wang Xia,Zhai Suyan,Liu Chao,Wang Xiaoshu,Yang Ya,Tu Yifeng
An antibody-based immunotherapy for methamphetamine (MA) addictive treatment is has been drawing more and more attention in recent years. However, studies about methamphetamine antibody (anti-MA) immunodetections are rare, owing to the lack of immunogenicity of small molecule MA. This study provides a simple and effective approach to develop a convenient electrochemiluminescent (ECL) immunosensor for the testing of anti-MA. In short, the synthetic holoantigen of MA is immobilized on a homemade gold nanoparticles modified electrode as the sensing host for the specific recognition and detection of anti-MA. The research suggested, under optimal experimental conditions, the ECL intensity on resultant immunosensor has a wide-linear regression toward the anti-MA quantity within the range from 0.03 to 3.07 ng with a detection limit of 2.32 pg. It responded to the dosage of anti-MA in spiked blood samples with satisfactory recovery. According to the research, the developed sensor shows promise as a portable Anti-MA fast seized device which performs quickly and offers convenience, and will be helpful for forensic identification and clinical treatment.
研究领域:
分析化学
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生物医学工程
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法医学
·
药物成瘾研究
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ENVIRONMENTAL POLLUTION
·
2024
·
IF 7.6
Lijuan Luo,Junhui Wu,Xueting Yuan,Xinyan Li,Bi Huang,Shanshan Chen,Jiewei Deng,Tiangang Luan
Psychoactive substances abuse is a global issue, with the methamphetamine (METH) being the most used and produced illicit substance in recent years. METH has been recognized as emerging contaminants in aquatic ecosystems. Research on the removal of METH from surface water is still lacking in-depth exploration. The effects of key aqueous environmental factors on the photodegradation of METH were investigated in this study. NO₃ ⁻ , Fe 3+ and dissolved organic matter (DOM) enhanced the photodegradation of METH, respectively, with degradation rates increasing as their concentrations increased. When HCO₃ ⁻ coexisted with NO₃ ⁻ , it exhibited dual effects on METH photodegradation: low concentrations inhibited the process, whereas high concentrations promoted it. The primary photodegradation products of METH, such as OH-METH, (OH) 2 -METH, AMP and NO 2 -OH-METH, were identified. The latter two compounds were newly discovered in this study. The mechanism of NO₃ ⁻ , HCO₃ ⁻ and Fe 3+ accelerating the photodegradation of METH in water was proposed to proceed via the generation of hydroxyl radical (HO∙), leading to the oxidation of METH, along with the involvement of nitro radical (∙NO 2 ) and carbonate radical (CO 3 •- ).
研究领域:
环境科学
·
化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ENVIRONMENTAL SCIENCE AND POLLUTION RESEARCH
·
2022
·Vol. 29
·期 40
·60244-60258
·
IF 5.19
Li Jianmin,Han Jiahua,Lan Tingting,Mu Shiyin,Hu Deyu,Zhang Kankan
The hydrolysis and photolysis of the chiral fungicide mandipropamid were investigated, and the potential enantioselectivity of mandipropamid in solutions was further assessed. The aqueous solutions were filtered and directly injected into the liquid chromatography with tandem mass spectrometry. In the hydrolysis experiments, mandipropamid enantiomers hydrolyzed slowly in aquatic solutions with half-lives > 200 days; nevertheless, rise of the pH and incubation temperature could increase the hydrolysis rates more than 1.1 times (half-lives decreased from 495.1 to 216.6 days). Compared with the hydrolysis results, photolysis was found to be the main degradation pathway for mandipropamid in different solutions (half-lives < 14 h, except in pH = 5.05 buffer solution). Organic solvents were able to accelerate the photolysis of mandipropamid, but acidic solutions and the addition of flavonoids or inorganic salts significantly inhibited the photolysis of mandipropamid. During the hydrolysis and photolysis processes, the configuration of mandipropamid enantiomers was stable and five possible transformation products were identified by high resolution mass spectrometry. Due to the enantiomeric fraction values > 0.5, the hydrolysis and photolysis of mandipropamid were enantioselective, and S -( +)-mandipropamid preferentially disspated in certain aqueous solutions. The systematic evaluation of the hydrolysis and photolysis of mandipropamid enantiomers may provide more accurate data for better assessment of environmental and ecological risks in aquatic ecosystems. Graphical abstract
研究领域:
环境科学
·
分析化学
✓ 已验证
DOI
PubMed
高影响因子
Nano Research
·
2018
·Vol. 11
·期 3
·1447-1455
·
IF 7.994
Cai Zhixiong,Li Feiming,Xu Wei,Xia Shujun,Zeng Jingbin,He Shaogui,Chen Xi
Perovskite nanocrystals (NCs), which have emerged as a new class of phosphors with superb luminescence properties and bandgaps that can be easily tuned using chemical methods, have generated tremendous interest for a wide variety of applications where colloidal quantum dots have been very successful as carrier sources. In this study, self-assembled films of CsPbBr 3 NCs were produced via drop casting of colloidal NCs onto glassy carbon electrodes (GCEs) to form an NC film-modified electrode. The possible fabrication process of the CsPbBr 3 NCs films was discussed. We further studied the anodic electrochemiluminescence (ECL) behavior of the perovskite CsPbBr 3 NCs film using cyclic voltammetry with tripropylamine (TPA) as a coreactant, and a possible ECL mechanism was proposed. Briefly, TPA was oxidized to produce strongly reducing radical species, which can react with electrochemically oxidized CsPbBr 3 NCs to generate excited CsPbBr 3 NCs* capable of light emission. The relative stability of the ECL emission of the CsPbBr 3 NC films under aqueous conditions was also investigated, and it was found that they showed operational stability over the first three hours, indicating suitable reliability for application as sensing materials. The results suggested that semiconducting perovskite NCs have great potential for application in the ECL field.
研究领域:
材料科学
·
电化学
✓ 已验证
产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）