Water
·
2024
·Vol. 16
·期 9
·1315
·
IF 3
Kan Li,Yiling Hu,Yuke Jiang,Xing Han,Xin Liu,Mingluo Du
The determination of illegal drugs and psychoactive substances in wastewater is increasingly being used to monitor the use of both by populations in specific areas. This article describes a method for the simultaneous determination of 78 illegal drugs and psychoactive substances in wastewater using direct-injection ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). This method includes the analysis of stimulants, opioids, antidepressants, antipsychotic drugs, anti-anxiety drugs, and hallucinogens. The method was validated in terms of the selectivity, calibration range, recovery, matrix effects, accuracy, precision, limit of detection (LOD), and limit of quantification (LOQ). The correlation coefficients were higher than 0.99 for all analytes, and the calibration range was from 0.2 to 500 ng/L. The LOD and LOQ of this method were 0.1–1 ng/L and 0.2–5 ng/L, respectively. The intra- and inter-day precisions were <9.3% and 11.4%, respectively, and the recovery ranged from 81.3% to 117.7%. The method was applied to real domestic wastewater collected from wastewater treatment plants, and the results showed that morphine, codeine, and ephedrine were detected in all samples. Some samples also contained other illegal drugs and psychoactive substances (such as etomidate, methamphetamine, ketamine, and tramadol). This indicates that the direct-injection UHPLC-MS/MS method can be used for the rapid determination of illegal drugs and psychoactive substances in wastewater.
研究领域:
环境科学
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分析化学
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毒理学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Liangming Luo,Chenlu Wang,Yong Wu,Hao Zhang,Feng Xu,Keqi Tang,Jiancheng Yu
Screening for illicit drugs in urban wastewater provides an important tool for monitoring and tracing the use of illicit drugs, increasingly leaning towards on-site detection of wastewater samples. This study established an on-site detection method for three illicit drugs—ketamine (KET), cocaine (COC), and codeine(COD)—in wastewater, based on an automatic solid-phase extraction device and a portable mass spectrometer. After enrichment and purification of samples using HLB solid-phase extraction cartridges, a portable mass spectrometer equipped with a sub-atmospheric pressure chemical ionization source was used for quantitative analysis of target drugs in selected ion monitoring mode. The solid-phase extraction conditions and parameters of the subatmospheric pressure chemical ionization source were studied and optimized, and the method was evaluated. The results showed that ketamine, cocaine, and codeine exhibited good linearity (R² > 0.99) within the concentration range of 1∼40 μg/L, with limits of detection (LODs) of 0.30∼0.42 μg/L. The recoveries were between 70.52% and 118.56%. This method can be used for on-site rapid screening of illicit drugs in wastewater. Compared to traditional laboratory analysis methods, it reduces sample transportation and storage costs, shortens the detection cycle. Finally, evaluations based on GAPI, AGREE, and BAGI indicators indicated that this method could serve as a green alternative for the screening of illicit drugs in wastewater.
研究领域:
环境科学
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分析化学
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DOI
PubMed
高影响因子
Drug Testing and Analysis
·
2020
·Vol. 13
·期 3
·720-728
·
IF 2.903
Cui-Mei Liu,Hong-Yuan He,Lin Xu,Zhen-Dong Hua
Performing fast qualitative identification of seized illegal drugs by Raman spectroscopy is challenging due to fluorescence interference as well as chemical complexity. Spectrometers with 785-nm excitation, 1,064-nm excitation, and sequentially shifted excitation (SSE) were compared for their effect on fluorescence reduction. The characteristic peaks method, which is independent of cutting agents, was tested as a new strategy to broaden the application of the Raman technique. The suitability of the characteristic peaks method was fully examined by analyzing a large amount of seized illegal drugs, including 72 methamphetamine hydrochloride (concentration range of 13.9%–99.4%), 68 ketamine hydrochloride (17.7%–99.8%), 176 heroin hydrochloride (5.2%–79.5%), 51 cocaine hydrochloride (21.1%–94.5%), and 33 cocaine base (30.9%–92.5%) samples. The results showed that seized methamphetamine, ketamine, and cocaine samples had no or little fluorescence. Hence, in regard to detection of these samples, the advantage of using 1,064-nm excitation and SSE compared with 785-nm excitation was quite limited. Regarding the heroin samples, a significant improvement of the “high” confident positive detected rate was evident for 1,064 nm excitation (60.8%) and SSE (61.4%), compared with 785-nm excitation (13.1%). However, it was also seen that even if 1,064-nm excitation and SSE were applied, the fluorescence of heroin samples was still unable to be fully overcome. By using the characteristic peaks method, low LOD results of 5%–20% were acquired for 40 types of drug mixtures, and lower LODs were obtained for the 60% of the drug mixtures compared with library searching method. Raman spectroscopy in conjunction with the characteristic peaks method was shown to be fast, simple, accurate, and sensitive in the qualitative analysis of seized drug samples.
研究领域:
分析化学
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法医学
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DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
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2024
·
IF 4.9
Linzhou Chen,Jiedan Zhou,Yuesen shi,Fei Xu,Xin Liu,Qingda Huang,Jinjian Zhong,Ke Wu,Dafeng Yang,Huajun Fan,Xiangliang Yang
Collecting exhaled breath aerosols (EBA) as a sample has a great potential to monitoring illicit drug abuse due to advantages of simple, non-invasiveness and unrestricted sampling. However, scarcity of positive samples has cramped development of more efficient techniques for monitoring illicit drug abuse in EBA. In this work, a simulated human exhaled breath aerosol (SHEBA) generating device based on Venturi jet principle was constructed by integrating nebulizing unit and collection unit to prepare positive EBAs. By means of ultra high-performance hyphenated with triple quadrupole tandem mass spectrometry (HPLC-TQ-MS/MS), using caffeine as a target drug, the device parameters were investigated by studying the effects of flow rates of nebulizing and auxiliary gases, drug concentration and etc., the performance was further validated by commonly abused drugs such as amphetamines (AMP, MAMP, MDA and MDMA). Electret material as adsorbent was used to collect SHEBAs generated by the device, achieving HPLC-TQ-MS/MS detection of the captured drugs at 40.0–2000.0 pg/filter. By this way, caffeine content in EBAs from six volunteers was successfully detected in the range of 51.6 ± 6.8–708 ± 51 pg/filter after drinking the caffeinated beverage. These validation experiments proved that SHEBA generating device could not only meet to the requirement of EBA analysis for illicit drug abuse at trace levels, but also provide the correction factors to calibrate the lower detection value caused by incomplete material adsorption.
研究领域:
分析化学
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毒理学
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医学检测
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DOI
高影响因子
WATER SCIENCE AND TECHNOLOGY
·
2020
·Vol. 82
·期 9
·1771-1780
·
IF 1.638
Yuan Shuai,Wang Xin,Wang Roujia,Luo Ruxin,Shi Yan,Shen Baohua,Liu Wei,Yu Zhiguo,Xiang Ping
Assessing collective drug consumption based on the concentrations of illicit drugs and their metabolites in wastewater is a new technology. Currently, this technology is receiving attention in China, and methods for multiple illicit drug detection in wastewater are urgently needed. In our study, a method with a short runtime (7 min), a small solid-phase extraction (SPE) loading volume (50 mL) and high sensitivity (lower limits of quantitation (LLOQs) ranged from 0.2 to 5 ng/L) was developed for the simultaneous determination of amphetamines, ketamine, opiates, cocaine and their metabolites in wastewater. Samples were enriched by SPE on a mixed-mode sorbent (Oasis MCX) and analyzed by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The limits of detection (LODs) ranged from 0.1 to 2 ng/L, and the LLOQs varied between 0.2 and 5 ng/L. Moreover, the method developed was applied to real wastewater samples collected from 15 different wastewater treatment plants (WWTPs). In the results, the most abundant compounds were morphine (1.8–46.6 ng/L) and codeine (3.7–24.9 ng/L), which were detected in 13 WWTPs. After successful optimization of the UPLC-MS/MS conditions and sample loading pH, the method developed is able to meet the needs of common illicit drug monitoring and high-throughput analysis requirements. SPE-UPLC-MS/MS method was developed for the for determination of 11 illicit drugs in wastewater. The method has a smaller SPE loading volume, a shorter UPLC runtime and higher sensitivity than other methods. The method can meet the requirements for current drug abuse monitoring in China.
研究领域:
分析化学
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环境科学
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药物滥用监测
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Shuai Yuan,Yangjiayi Xiang,Lizhu Chen,Ping Xiang,Yan Li
The quantification of illicit drugs in wastewater has become a valuable tool for monitoring illicit drug abuse. The commonly utilized methods for detecting drugs in wastewater require a substantial sample volume, extended pretreatment durations, and intricate procedures. This study first employed polydopamine-coated magnetic nanocomposites as adsorbents for magnetic solid-phase extraction, combined with UPLC-MS/MS, to simultaneously determine the concentrations of eleven common illicit drugs in wastewater. The synthesis process for Fe 3 O 4 @PDA is straightforward and high-yield. Benefiting from the strong magnetic response, good dispersibility, and abundant binding sites of the prepared nanocomposites, the extraction of illicit drugs from wastewater could be achieved in just 15 min. The method exhibited satisfactory limits of quantitation (ranging from 5 to 10 ng/L), commendable accuracy (ranging from 90.59 % to 106.80 %), good precision (with RSDs below 10 %), and less sample consumption (only 1 mL). The efficacy of this method was successfully validated through its application to actual wastewater samples collected from ten wastewater treatment plants. The results indicated that morphine, codeine, methamphetamine, and ketamine were the predominant illicit drugs present in the samples. The method developed is able to meet the needs of common illicit drug monitoring and high-throughput analysis requirements.
研究领域:
环境科学
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分析化学
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DOI
PubMed
高影响因子
ANALYTICAL LETTERS
·
2023
·
IF 2
Shifu Hu,Jiancheng Yu,Jun Li,Xu Tang,Keqi Tang
With the increasing prevalence of illicit drugs, social security and human health are at serious risk. However, traditional detection techniques require a lengthy pretreatment process to eliminate matrix interference and do not allow rapid, in situ analysis. Ambient ionization is a powerful tool for the rapid determination of illicit drugs in different matrices because it usually eliminates the need for sample pretreatment, and the portable mass spectrometer brings convenience to in situ detection. This study employed a thermal desorption-electrospray ionization (TD-ESI) source combined with a portable mass spectrometer to rapidly characterize illicit drugs in drinks, instant powders, and solid food surfaces. Air was utilized instead of nitrogen as the carrier gas for TD-ESI/MS in order to save space and cost together with rapid on-site analysis. A full-scan waveform combined with a qualitative pre-scan waveform (QPSW) was employed to form a two-step scanning mode to accurately identify the drugs. The results showed that the limits of detection (LODs) for the analytes were 100–200 ppb in drinks, 700–1000 ppb in instant powders, and 1 ng/cm2 on solid food surfaces. The complete TD-ESI/MS analysis time was less than 1 min.
研究领域:
分析化学
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法医学
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公共安全
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DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2022
·
IF 3.571
Likai Qi,Xinyi Jiang,Ning Wu,Jingjing Li,Bin Di,Fang Yan
In this study, a novel polydopamine and C 18 dual-functionalized magnetic core-shell mesoporous silica (Fe 3 O 4 @nSiO 2 @mSiO 2 @PDA-C 18 ) nanocomposite was designed and synthesized, which was employed as an adsorbent to extract illegal drugs from urine samples by magnetic solid-phase extraction (MSPE) procedures. The as-prepared nanocomposite was fully characterized and combined with ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) to monitor 12 trace illegal drugs and metabolites, including 6-monoacetylmorphine (6-MAM), morphine (MOR), codeine (COD), amphetamine (AMP), methamphetamine (MAMP), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), ketamine (KET), norketamine (NK), cocaine (COC), benzoylecgonine (BZE) and methcathinone (MC). Optimal MSPE procedures were achieved by fully investigating parameters of activation, adsorption, washing and desorption steps. The MSPE-UHPLC-MS/MS method offered high sensitivity with limit of detection (LOD) range of 0.005–0.05 ng mL -1 and good linearity with the concentration of 0.01–1000 ng mL -1 . Also, the intra- and inter-day recovery respectively ranged in 90.2–105.0% and 89.8–107.4%, and the intra- and inter-day precision was in the range of 0.5–14.0% and 1.2–10.0%, respectively. By application to real urine samples, the proposed method could not only be equally sensitive for quantifying 12 illegal drugs in urine but also significantly reduce the pretreatment time when comparing with methods based on solid-phase extraction. Furthermore, the designed dual-functionalized adsorbents could also be applied for on-site determination of MAMP in urine coupled with urine test kit, and the detection threshold of MAMP urine test kit remarkably reduced from 1000 ng mL -1 to 50 ng mL -1 . Therefore, the present method was a convenient, economic and sensitive approach for determining illegal drugs in urine samples both on site and in the laboratory.
研究领域:
分析化学
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法医学
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DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2022
·
IF 4.601
Hongyu Ning,Yilei Fan,Huijun Liu,Zhongping Huang,Xing Ke,Yu Xu,Yuanbin She
A novel mixed-mode weak cation-exchange sorbent (PS-DVB-WCX-II) was prepared by the modification of polystyrene-divinylbenzene with mercaptosuccinic acid for the selective extraction of illicit drugs in environmental water. The PS-DVB-WCX-II was synthesized through the Friedel-Crafts acylation reaction on the surface of polystyrene-divinylbenzene, followed by nucleophilic substitution reaction and thiol-ene click reaction. The sorbent can selectively absorb illicit drugs through the reverse-phase interactions provided by benzene ring on the polymer backbone and the ion-exchange interactions provided by functional group (-COOH). As compared with the extraction performance of three commercial SPE cartridges, it was found that the prepared sorbent had better adsorption performance with the recovery values between 84.1% and 106.0% for the selected 11 illicit drugs under the optimized SPE conditions. Illicit drugs in environmental water were extracted by the sorbent, prior to the detection of UHPLC-MS/MS. Two quantitative methods were established respectively for the detection of 11 illicit drugs in different matrices of river water and wastewater. Both methods had good determination coefficient (r 2 >0.992) in the range of 0.5–50 ng/L, 2.5–250 ng/L, 5–500 ng/L, and low limits of detection ( S / N = 3) of 0.17–1.67 ng/L. In the real wastewater samples, the concentration of morphine was 18.3–126.3 ng/L, and the methamphetamine was 12.7–27.4 ng/L. Meanwhile, PS-DVB-WCX-II was compared with Oasis MCX and Oasis HLB in the detection of real wastewater samples. The results revealed that PS-DVB-WCX-II and Oasis MCX had better performance in absorbing methamphetamine than Oasis HLB, and PS-DVB-WCX-II had better ability to remove the matrix. The results suggested that the prepared weak cation-exchange sorbent had the potential in the application of illicit drug detection in environmental water.
研究领域:
分析化学
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环境科学
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DOI
PubMed
高影响因子
Heliyon
·
2024
·
IF 3.4
Shunqin Chen,Han Yang,Shan Zhang,Faze Zhu,Shan Liu,Huan Gao,Qing Diao,Wenbo Ding,Yuemeng Chen,Peng Luo,Yubo Liu
This study developed an online solid-phase extraction ultra-high performance liquid chromatography-tandem mass spectrometry (Online-SPE-UHPLC-MS/MS) method for the analysis of 28 illegal drugs in sewage. To achieve this, 28 isotope internal standards (ISTDs) were added to 3 mL sewage samples, the pH was adjusted to 7–8 using hydrochloric acid or 20% ammonia water, followed by centrifugation, filtration, and analysis using UHPLC-MS/MS. The results indicated an excellent linearity of 1–300 ng L −1 , and cotinine in the concentration range of 20–6000 ng L −1 , linear correlation coefficient R 2 > 0.995, with the limit of detection (LOD) of 0.01–6 ng L −1 , and a limit of quantification (LOQ) of 0.1–20 ng L −1 . The addition of three concentrates of low (2 ng L −1 /40 ng L −1 ), medium (20 ng L −1 /400 ng L −1 ), and high concentration (200 ng L −1 /4000 ng L −1 ) demonstrated the matrix effect of the target compound between ± 22.0%. The extraction recovery was 70.0–119.4%, and a percent accuracy of 75.7–118.1%. Similarly, the intra- and inter-day precisions were 1.8–20.0% and 1.5–18.9%, respectively. The results cemented the sensitivity, accuracy, reliability, strong specificity, and reproducibility, which can be used to screen 28 illegal drugs in sewage for trace analysis.
研究领域:
环境科学
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分析化学
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毒理学
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DOI
PubMed
高影响因子
TOXICOLOGY LETTERS
·
2022
·
IF 4.271
Shiqi Duan,Yan Jia,Zhihang Zhu,Lancheng Wang,Peng Xu,Youmei Wang,Bin Di,Chi Hu
Information regarding the metabolism of illicit drugs is under urgent need for toxicological assessment . Its development, however, is limited by the currently available animal models. To this end, we proposed three-dimensional (3D) HepaRG spheroids as an in vitro model to study the effects of illicit drugs on hepatic cytochrome P450 (CYP450) enzymes and potential drug-drug interactions (DDIs). By comparing the results from animal and cell experiments, we confirmed the significant impact of heroin, morphine, tetrahydrocannabinol , and fentanyl on CYP450 enzymes, and the 3D spheroids results were in good agreement with the animal results for 2B6, 2C19, 2D6. Using 3D HepaRG spheroids, we demonstrated DDIs between heroin as a 2B6 perpetrator and clinical medicine for cancer, depression, and illicit drug withdrawal. Specifically, the clearance rate of 5.4 μM bupropion was increased by 214 % under DDI with 5 µM heroin, highlighting the importance of DDI pre-screening and individualized medication guidance for illicit drug users. This research contributes to the growing body of evidence regarding the metabolic toxicity of illicit drugs and suggests 3D HepaRG spheroids as a high-throughput and cost-efficient platform for DDI analysis.
研究领域:
药理学
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毒理学
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细胞生物学
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药物代谢
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DOI
PubMed
高影响因子
ANALYST
·
2019
·Vol. 144
·期 24
·7406-7411
·
IF 4.019
Pan Li,Huan He,Dongyue Lin,Liangbao Yang
A rapid and accurate method for the sensitive detection of illegal drug additives including atenolol (ATN), metformin hydrochloride (MET), and phenformin hydrochloride (PHE) in health products using solvent microextraction (SME) combined with surface-enhanced Raman spectroscopy (SERS) was developed. Various illegal drug additives in different health products were separated via microextraction and then detected in situ using a portable Raman spectrometer with Ag colloids acting as SERS-active substrates. The effects of experimental parameters on the detection sensitivity and producibility were evaluated, and the applications of illegal additives spiked into samples were systematically investigated with SME-SERS. It was demonstrated that the mixture of CH3OH and CHCl3 (v/v = 1 : 4) as the extractant was suitable for the rapid microextraction separation of illegal drug additives and also induced the distribution of the Ag colloids (2 M) on the CHCl3 surface. More importantly, CH3OH can carry the drug molecules to enter into the inter-particles of the Ag colloids in this process, and then significantly improve the detection sensitivity of illegal drug additives. Furthermore, the high-throughput and real-time detection of illegal drug additives spiked into health products with SME-SERS in multi-well 96 plates were achieved with the level of 0.1 μg mg−1. The results reveal that this rapid and convenient method could be used for the effective separation and sensitive detection of illegal additives in complex specimen.
研究领域:
分析化学
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药学
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光谱学
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DOI
PubMed
高影响因子