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Robust provenance classification of curcumae radix (Yujin) using nir-hsi: Preprocessing, nested CV and morphology effects 基于nir-hsi的姜黄种源稳健分类:预处理、嵌套CV和形态效应
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-29 DOI: 10.1016/j.microc.2026.117170
Yujia Dai, Haoyuan Ding, Shangyong Zhao, Ziyuan Liu
We evaluated near-infrared hyperspectral imaging in the range of 900–1700 nm combined with machine learning for geographic origin authentication of Curcumae Radix collected from six major Chinese production regions. Each origin was represented by 100 specimens measured both as intact root slices and as finely milled powder. Three classification algorithms—support vector machine, random forest, and k-nearest neighbor—were compared after five common spectral preprocessing methods, using stratified train–test splits and nested cross-validation to ensure reliable generalization estimates. Model robustness was further assessed through per-origin holdout testing, permutation analysis, and the introduction of Gaussian noise and illumination variation, along with bootstrap-derived confidence intervals. Support vector machine consistently achieved the highest performance, with root slices reaching an average accuracy of 95.17% and powders achieving 99.00%. Powder spectra demonstrated not only higher discriminative power but also greater resilience to measurement noise and lighting changes compared with intact-root spectra. These results indicate that morphology-aware preprocessing combined with SVM enables rapid, non-destructive, and statistically validated provenance identification of Yujin, with powder-based assays offering the optimal balance between accuracy, robustness, and operational efficiency.
利用900 ~ 1700 nm波段的近红外高光谱成像技术,结合机器学习技术,对中国6个主要产区的姜黄进行了产地鉴定。每个产地都有100个标本,包括完整的根片和磨细的粉末。在五种常见的光谱预处理方法后,使用分层训练测试分割和嵌套交叉验证来确保可靠的泛化估计,对支持向量机、随机森林和k近邻三种分类算法进行了比较。模型的稳健性通过每个原点的保留检验、排列分析、高斯噪声和光照变化的引入以及自举推导的置信区间进一步评估。支持向量机始终取得了最高的性能,根片的平均准确率达到95.17%,粉末的平均准确率达到99.00%。与完整根光谱相比,粉末光谱不仅具有更高的分辨能力,而且对测量噪声和光照变化具有更强的适应能力。这些结果表明,形态感知预处理与支持向量机相结合,可以快速、无损、统计验证玉金的来源识别,而基于粉末的分析在准确性、鲁棒性和操作效率之间取得了最佳平衡。
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引用次数: 0
A novel procedure for the detection of personal care products (PCPs) in outdoor air: Occurrence in urban, coastal, alpine, and polar areas 一种检测室外空气中个人护理产品(pcp)的新方法:发生在城市、沿海、高山和极地地区
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-29 DOI: 10.1016/j.microc.2026.117159
Marco Vecchiato , Giorgia Trevisanato , Diego Costa , Elena Barbaro , Marianna D'Amico , Giovanna Mazzi , Andrea Gambaro
Personal care products (PCPs) are compounds largely emitted and detected in the water compartment. However, as emerged in recent literature, their presence in the atmosphere is fundamental to understanding their environmental fate. Standardized procedures for the determination of PCPs in the atmosphere are still lacking. We developed a new analytical method to determine fragrances and UV filters in outdoor samples, focusing on their distribution both in the gas (Polyurethane foam; PUF) and Total Suspended Particulate (TSP; quartz filter) phases. A low-temperature (40 °C) solvent extraction procedure was adopted, followed by GC–MS/MS instrumental analyses. The method was tested on samples collected during summer 2023 in low and high anthropogenic-impacted sites: urban, coastal, and alpine areas of the Veneto Region in Italy, and a remote area in the Norwegian Arctic (Ny-Ålesund, Svalbard). Results showed the highest levels of ΣPCPs near the seashore (13–16 ng m−3), reflecting the widespread use of sunscreen products in summer by touristic and recreational activities. Lower concentrations were observed in the urban area (ΣPCPs = 6.0–8.5 ng m−3), followed by the alpine samples from the Dolomites (ΣPCPs = 1.6–3.0 ng m−3). In the Arctic, ΣPCPs were orders of magnitude lower (0.11–1.3 ng m−3) compared to the other sites. Among PCPs, Galaxolide, Tonalide and Ethylene Brassylate were generally the main musk fragrances, while Salicylates were the most abundant compounds among UV filters and non-musk fragrances. The selected PCPs were mainly distributed in the gas phase, with the exception of Octocrylene. This agrees with previous hypotheses and findings that associate this UV filter with the atmospheric particulate. The analytical method presented in this study will contribute to further understanding the behavior of PCPs in the atmosphere and to assess their long-range transport.
个人护理产品(pcp)主要是化合物释放和检测在水隔间。然而,正如最近文献中出现的那样,它们在大气中的存在是了解其环境命运的基础。目前仍缺乏测定大气中pcp的标准化程序。我们开发了一种新的分析方法来确定室外样品中的香料和紫外线过滤器,重点关注它们在气相(聚氨酯泡沫;PUF)和总悬浮颗粒(TSP;石英过滤器)中的分布。采用低温(40°C)溶剂萃取,GC-MS /MS仪器分析。该方法在2023年夏季在低和高人为影响地点收集的样本上进行了测试:意大利威尼托地区的城市、沿海和高山地区,以及挪威北极的偏远地区(Ny-Ålesund,斯瓦尔巴群岛)。结果显示,沿海地区的ΣPCPs水平最高(13-16 ng m - 3),反映了夏季旅游和娱乐活动普遍使用防晒产品。城市地区的浓度较低(ΣPCPs = 6.0 ~ 8.5 ng m−3),其次是白云岩的高山样品(ΣPCPs = 1.6 ~ 3.0 ng m−3)。在北极,ΣPCPs比其他地点低了几个数量级(0.11-1.3 ng m−3)。在pcp中,麝香成分以Galaxolide、Tonalide和乙烯Brassylate为主,而水杨酸盐是紫外线过滤器和非麝香成分中含量最多的化合物。所选pcp除奥克力外,主要分布在气相中。这与之前的假设和发现一致,即紫外线过滤器与大气微粒有关。本研究提出的分析方法将有助于进一步了解pcp在大气中的行为并评估其远程传输。
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引用次数: 0
Porous tube Sorptive extraction: A robust sol–gel sorbent encapsulated device for monitoring bisphenols in human urine 多孔管吸附萃取:一种用于监测人体尿液中双酚类物质的溶胶-凝胶吸附封装装置
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-29 DOI: 10.1016/j.microc.2026.117161
Pavlos Voutsas , Konstantinos Angeli , Abuzar Kabir , Fernando Zaldivar Eyre , Natasa Kalogiouri , Victoria Samanidou
Α new microextraction platform Porous Tube Sorptive Extraction (PTSE) is reported for the first time for the selective isolation of bisphenols from human urine prior to HPLC–DAD analysis. The novel device consists of a micro-porous tubular substrate uniformly coated with a sol–gel Polyethylene Glycol 20 K (sol-gel PEG 20 K) sorbent phase, providing a high surface area, hydrophilic–lipophilic network that promotes efficient partitioning of target analytes while minimizing matrix effects. Key operational variables were optimized using a one-factor-at-a-time (OFAT) strategy, and the PTSE–HPLC–DAD workflow was validated in human urine. The method delivered high recoveries (71.0–100.9%), good linearity across the working range, and low quantitation and detection limits of 0.05 ng/μL and 0.015 ng/μL, respectively. The PTSE device operated with minimal organic solvent and supported multiple extraction-desorption cycles without appreciable loss of performance, underscoring its robustness and cost-efficiency. Method greenness was quantitatively confirmed using Modified Green Analytical Procedure Index (MoGAPI) and Blue Applicability Grade Index (BAGI) metrics, evidencing reduced solvent consumption and waste generation relative to conventional approaches. Overall, PTSE combines selectivity, sensitivity, and sustainability in a compact format compatible with routine HPLC–DAD analysis, positioning it as a practical tool for bisphenol biomonitoring and a promising template for future sol–gel tube-based microextraction devices.
Α新微萃取平台多孔管吸附萃取(PTSE)首次报道了在HPLC-DAD分析之前从人尿中选择性分离双酚类物质的方法。该新型装置由微孔管状基底组成,均匀涂有溶胶-凝胶聚乙二醇20k(溶胶-凝胶PEG 20k)吸附剂相,提供高表面积,亲水亲脂网络,促进目标分析物的有效分配,同时最大限度地减少基质效应。使用单因素-一次(OFAT)策略对关键操作变量进行了优化,并在人尿中验证了pse - hplc - dad工作流程。该方法回收率高(71.0 ~ 100.9%),在工作范围内线性良好,定量限和检出限分别为0.05 ng/μL和0.015 ng/μL。PTSE设备使用最少的有机溶剂,并支持多次萃取-解吸循环,而不会出现明显的性能损失,强调了其稳健性和成本效益。采用改进的绿色分析程序指数(MoGAPI)和蓝色适用性等级指数(BAGI)指标定量确认方法的绿色度,证明相对于传统方法减少了溶剂消耗和废物产生。总的来说,PTSE结合了选择性、敏感性和可持续性,其紧凑的格式与常规HPLC-DAD分析兼容,将其定位为双酚生物监测的实用工具和未来基于溶胶-凝胶管的微萃取设备的有前途的模板。
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引用次数: 0
Sensitive PEC detection of alkaline phosphatase and organophosphorus pesticides via enzyme-catalyzed signal amplification on a CdS@in₂S₃ platform 在CdS@in₂S₃平台上通过酶催化信号放大对碱性磷酸酶和有机磷农药进行灵敏的PEC检测
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-29 DOI: 10.1016/j.microc.2026.117158
Xiaoying Liu , Yu Xie , Yuee Zhong , Jingshu Li , Meiling Liu , Youyu Zhang , Qiang Li
Alkaline phosphatase (ALP) is a critical biomarker for the diagnosis of various diseases. Consequently, the precise detection of ALP activity is indispensable for clinical diagnosis, biomedical research, and the screening of enzyme inhibitors. Meanwhile, organophosphorus pesticides (OPs), a class of highly toxic and persistent environmental contaminants, have raised significant concerns due to their extensive use in agriculture and their potential risks to both ecosystems and human health. Here, we developed a novel photoelectrochemical (PEC) biosensing platform based on an optimized CdS@In₂S₃ heterojunction for the detection of ALP activity and OPs compounds. Through systematic optimization of the In₂S₃ incorporation ratio, a significant enhancement in photoelectric conversion efficiency compared to pristine CdS was achieved. The sensing mechanism exploits the synergistic effects of the ALP mediated hydrolysis of L-ascorbyl-2-phosphate trisodium salt (AAP) to generate ascorbic acid (AA) and the AA-induced photocurrent amplification of the CdS@In₂S₃ heterojunction. This dual signal amplification strategy enabled ultrasensitive detection of ALP activity with a wide linear range of 0.17–17,000 U/L and an exceptionally low detection limit (LOD) of 0.0083 U/L. Chlorpyrifos (CPF) inhibits the activity of ALP, thereby reducing the amount of AA generated from AAP catalyzed by ALP. This results in attenuation of the AA-dependent photocurrent signal. By quantifying the degree of such photocurrent suppression, highly sensitive detection of CPF was achieved with a broad dynamic range of 0.1 ng/mL to 5 μg/mL and the LOD of 0.03 ng/mL. The sensor exhibited excellent operational stability (<5.5% RSD over 50 cycles), high selectivity against common interferents, and reliable performance in complex matrices (89–114% recovery in serum and agricultural samples). This work not only presents a robust analytical tool for food safety and biological monitoring but also provides new insights into the design of multifunctional heterojunction-based PEC sensors for dual-targets detection.
碱性磷酸酶(ALP)是诊断多种疾病的重要生物标志物。因此,ALP活性的精确检测对于临床诊断、生物医学研究和酶抑制剂的筛选是必不可少的。与此同时,有机磷农药是一类剧毒和持久性环境污染物,由于其在农业中的广泛使用及其对生态系统和人类健康的潜在风险而引起了重大关注。在这里,我们开发了一种基于优化的CdS@In₂S₃异质结的新型光电化学(PEC)生物传感平台,用于检测ALP活性和OPs化合物。通过系统优化In₂S₃混合比,实现了与原始cd相比光电转换效率的显著提高。该传感机制利用了ALP介导的l-抗坏血酸-2-磷酸三钠盐(AAP)水解生成抗坏血酸(AA)和AA诱导的CdS@In₂S₃异质结光电流放大的协同效应。该双信号放大策略可实现ALP活性的超灵敏检测,线性范围为0.17 ~ 17000 U/L,检出限(LOD)极低,为0.0083 U/L。毒死蜱(Chlorpyrifos, CPF)抑制了ALP的活性,从而减少了由ALP催化的AAP产生的AA量。这导致了依赖于aa的光电流信号的衰减。通过对这种光电流抑制程度的量化,实现了CPF的高灵敏度检测,动态范围为0.1 ng/mL ~ 5 μg/mL, LOD为0.03 ng/mL。该传感器具有良好的操作稳定性(50个周期内RSD为5.5%),对常见干扰物具有高选择性,在复杂基质中具有可靠的性能(血清和农业样品的回收率为89-114%)。这项工作不仅为食品安全和生物监测提供了一个强大的分析工具,而且为设计用于双靶标检测的多功能异质结型PEC传感器提供了新的见解。
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引用次数: 0
Precise classification of rice blast disease using an improved MCG-net with multi-feature fusion technology for UAV hyperspectral imagery 基于多特征融合技术的改进MCG-net无人机高光谱影像稻瘟病精确分类
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-28 DOI: 10.1016/j.microc.2026.117105
Tan Liu , Peiyan Wu , Songlin Guo , Yuan Qi , Jun Ma , Qingyun Yuan , Chunling Chen
Rice blast disease severely impacts rice yield and quality. However, quantitative research on early-stage grading and detection of rice blast disease still faces technical challenges. This study extracted and integrated multidimensional features from hyperspectral data, including spectral features, texture features (TFs), and structural features. By integrating texture features with vegetation cover (FVC) to construct vegetation texture indices (VTIs), we achieved refined quantification of vegetation structural parameters, significantly enhancing vegetation type recognition and classification accuracy. Simultaneously, we employed Pearson correlation coefficient combined with sequential backward selection (PCC_SBS) to screen spectrally sensitive bands. The proposed MCG-net model enables deep fusion of spectral features and VTIs. This model integrates 1DCNN, GRU, and multi-scale self-attention (MSSA) modules: 1DCNN extracts multi-scale local features using convolutional kernels with varying dilation rates; GRU captures sequential dynamics and long-term dependencies; MSSA reduces model dependence on noise and irrelevant information. Experiments validate MCG-net's exceptional performance in data fusion, primarily attributed to its robust feature learning capability. The multi-feature fusion model (PCC_SBS + VTIs) achieved optimal performance with an overall accuracy (OA) of 96.67% and a kappa value of 95.83%, significantly outperforming models relying solely on spectral features or TFs. In summary, deep learning models integrating multiple features can effectively enhance rice blast disease detection efficiency, providing an efficient technical solution for field control and food safety
稻瘟病严重影响水稻产量和品质。然而,稻瘟病早期分级和检测的定量研究仍面临技术挑战。本研究从高光谱数据中提取并整合多维特征,包括光谱特征、纹理特征和结构特征。通过将纹理特征与植被覆盖度(FVC)相结合构建植被纹理指数(VTIs),实现了植被结构参数的精细化量化,显著提高了植被类型识别和分类精度。同时,我们采用Pearson相关系数结合序列反向选择(PCC_SBS)筛选光谱敏感波段。提出的MCG-net模型实现了光谱特征和vti的深度融合。该模型集成了1DCNN、GRU和多尺度自关注(MSSA)模块:1DCNN使用不同膨胀率的卷积核提取多尺度局部特征;GRU捕获顺序动态和长期依赖关系;MSSA减少了模型对噪声和不相关信息的依赖。实验验证了MCG-net在数据融合方面的卓越性能,这主要归功于其强大的特征学习能力。多特征融合模型(PCC_SBS + VTIs)的总体准确率(OA)为96.67%,kappa值为95.83%,显著优于单纯依赖光谱特征或tf的模型。综上所述,综合多种特征的深度学习模型可以有效提高稻瘟病检测效率,为田间防治和食品安全提供高效的技术解决方案
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引用次数: 0
UHPLC-MS/MS detection and health risk assessment of triazole pesticides in dates cultivated in the UAE: Protecting consumer health 阿联酋红枣中三唑类农药UHPLC-MS/MS检测及健康风险评价:保护消费者健康
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-28 DOI: 10.1016/j.microc.2026.117160
Muhammad Usman , Muhammad Kamran Hakeem , Shaima Askar , Iltaf Shah , Tamilarasan Rajendran , Kilani Ghoudi , Mohammed A. Meetani
With the world's population growing significantly and the rising demand for food, food safety has become a serious concern for the public. To meet these demands, pesticides are used on a larger scale; however, their residues in dates may damage the human body, leading to a significant threat to food safety. Consequently, it is crucial to conduct routine monitoring of pesticides in date samples to ensure public safety. Here, a highly sensitive and highly accurate method for determining triazole pesticide residues in date fruit samples was developed using QuEChERS-based extraction followed by UHPLC-MS/MS analysis. A total of 50 collected date samples from marketplaces and small local farms throughout the UAE were analyzed. The method demonstrated strong linearity (R2 ≥ 0.993) and achieved a low limit of detection (1.10–1.48 μg/kg) andlimit of quantification (3.64–4.88 μg/kg). All the analyzed date samples had residues of triazoles, with six samples exceeding maximum residue limits, primarily for paclobutrazol and triticonazole, with concentration ranged from 1.7 to 14 μg/kg. The most frequently detected triazole was difenoconazole (54% detection rate), followed by paclobutrazol (28% detection rate). The health risk results showed that there is no risk to the consumer from the exposure of triazoles from dates for adults and children at the present level of contamination (Hazard Index <1). Overall, this method offers a reliable analytical tool that can support regulatory authorities in strengthening pesticide monitoring and food-safety control in the region.
随着世界人口的显著增长和对食品需求的不断增加,食品安全已成为公众严重关注的问题。为了满足这些需求,农药被更大规模地使用;然而,它们在枣中的残留可能对人体造成损害,对食品安全构成重大威胁。因此,对食枣样品中农药进行常规监测对保障公众安全至关重要。建立了基于quechers提取- UHPLC-MS/MS分析的高灵敏度、高准确度测定红枣样品中三唑类农药残留的方法。对从阿联酋各地的市场和小型当地农场收集的50个日期样本进行了分析。方法线性良好(R2≥0.993),低检出限(1.10 ~ 1.48 μg/kg)和定量限(3.64 ~ 4.88 μg/kg)。所有样品中均有三唑类残留,其中6个样品超过最大残留限量,主要为多效唑和三康唑,浓度范围为1.7 ~ 14 μg/kg。三唑类药物检出率最高的是异丙康唑(检出率54%),其次是多效唑(检出率28%)。健康风险结果表明,在目前的污染水平下,成人和儿童从枣中接触三唑对消费者没有风险(危害指数<;1)。总体而言,该方法提供了一种可靠的分析工具,可支持监管当局加强该地区的农药监测和食品安全控制。
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引用次数: 0
Electrodeposited polyaniline @ divinylbenzene-N-vinylpyrrolidone microspheres on stainless steel wire for solid-phase microextraction of organophosphorus pesticides in juice 不锈钢丝电沉积聚苯胺@二乙烯基苯- n -乙烯基吡咯烷酮微球用于果汁中有机磷农药的固相微萃取
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-28 DOI: 10.1016/j.microc.2026.117152
Yilei Huang , Yuwen Fang , Jie Wei, Min Chen, Yi Xu, Tianhui Jiao, Qingmin Chen, Xiaomei Chen
This study developed a novel probe for rapid extraction of organophosphorus pesticides (OPPs) in guava juice. The probe was prepared by electropolymerizing polyaniline (PANI)-doped divinylbenzene (DVB)-N-vinylpyrrolidone (NVP) microspheres on stainless steel wire, followed by a silicone sealant (SCS) coating. The porous PANI layer enhances stability, while the amphiphilic DVB-NVP microspheres and SCS coating reduce matrix interference. In direct-immersion solid-phase microextraction, the probe effectively enriched three OPPs (diazinon, parathion-methyl, and fenitrothion). Coupled with gas chromatography, the method showed a linear range of 0.05–300 μg/L, detection limits of 10.25–14.23 ng/L, and RSDs of 3.2–6.5%. After 60 extraction cycles, efficiency declined only 11.8–14.8%. Recoveries from guava juice ranged 84.2–98.7% (RSD < 5.2%), confirming excellent anti-fouling performance.
研究了一种快速提取番石榴汁中有机磷农药的新探针。探针是通过在不锈钢丝上电聚合聚苯胺(PANI)掺杂二乙烯基苯(DVB)- n -乙烯基吡啶酮(NVP)微球,然后涂上硅酮密封胶(SCS)制备的。多孔聚苯胺层增强了稳定性,而两亲性DVB-NVP微球和SCS涂层减少了基质干扰。在直接浸没固相微萃取中,探针有效富集了三种OPPs(二嗪农、甲基对硫磷和非硝硫磷)。结合气相色谱法,该方法线性范围为0.05 ~ 300 μg/L,检出限为10.25 ~ 14.23 ng/L, rsd为3.2 ~ 6.5%。60次萃取循环后,萃取效率仅下降11.8 ~ 14.8%。番石榴汁的回收率为84.2 ~ 98.7% (RSD < 5.2%),具有良好的防污性能。
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引用次数: 0
Comprehensive UPLC–MS/MS analysis of etomidate and its structural analogs with isomer separation: validation and application to authentic urine samples 依托咪酯及其结构类似物异构体分离的UPLC-MS /MS综合分析:验证及在真实尿样中的应用
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-28 DOI: 10.1016/j.microc.2026.117128
Xiaoyu Qian , Liying Zhou , Tangchenxi Qing , Sujing Zhang , Ping Xiang , Mengxiang Su , Hui Yan
Etomidate is a short-acting intravenous anesthetic, and its structural analogs have increasingly emerged as substances of abuse. In this study, a UPLC–MS/MS method was developed and validated for the simultaneous qualitative and quantitative determination of etomidate, etomidate acid, and 11 structural analogs (metomidate, propoxate, isopropoxate, butomidate, sec-butomidate, isobutomidate, tert-butomidate, TF-etomidate, 4F-etomidate, ABP-700, and 2,6-diCl-3F-etomidate) in urine. A major challenge was the chromatographic separation of six structural isomers (propoxate, isopropoxate and the four butomidate isomers), which was achieved using a Phenomenex Kinetex® Biphenyl 100 Å column (100 × 3.0 mm, 2.6 μm) with mobile phases consisting of (A) water containing 2 mmol/L ammonium formate and 0.01% formic acid and (B) methanol under optimized gradient conditions. The method showed excellent linearity within 1–50 ng/mL for most analytes and 10–500 ng/mL for etomidate acid. Limits of detection (LODs) and limits of quantification (LOQs) ranged from 0.5–5 ng/mL and 1–10 ng/mL, respectively. Precision and accuracy ranged from 1.8%–10.4% and −10.4%–8.9%, respectively. Matrix effects were 89.6%–119.7%, and recoveries were 70.1%–98.7%. Application to 37 authentic urine samples revealed frequent detection of isopropoxate (n = 35), metomidate (n = 33), and etomidate (n = 34), while etomidate acid exhibited the highest concentrations (up to 31.2 μg/mL). Overall, this study provides a reliable, isomer-resolved analytical workflow for the determination of multiple etomidate analogs in urine samples.
依托咪酯是一种短效静脉麻醉剂,其结构类似物越来越多地被滥用。本研究建立并验证了UPLC-MS /MS方法,用于同时定性和定量测定尿中依托咪酯、依托咪酯酸和11种结构类似物(甲咪酯、丙酸酯、异丙酸酯、丁咪酯、异丁咪酯、叔丁咪酯、tf -依托咪酯、4f -依托咪酯、ABP-700和2,6- dicl - 3f -依托咪酯)。主要的挑战是六种结构异构体(丙酸酯、异丙酸酯和四种丁咪酯异构体)的色谱分离,使用Phenomenex Kinetex®Biphenyl 100 Å色谱柱(100 × 3.0 mm, 2.6 μm),流动相由(A)含2 mmol/L甲酸铵和0.01%甲酸的水和(B)甲醇组成,在优化的梯度条件下。方法在1 ~ 50 ng/mL范围内线性良好,对依托咪酯酸在10 ~ 500 ng/mL范围内线性良好。检出限(lod)为0.5 ~ 5ng /mL,定量限(loq)为1 ~ 10ng /mL。精密度和准确度范围分别为1.8%-10.4%和- 10.4%-8.9%。基质效应为89.6% ~ 119.7%,回收率为70.1% ~ 98.7%。应用于37份真实尿液样本,发现经常检测到异丙酸(n = 35),美托咪酯(n = 33)和依托咪酯(n = 34),其中依托咪酯酸的浓度最高(高达31.2 μg/mL)。总的来说,本研究为尿液样本中多种依托咪酯类似物的测定提供了可靠的,异构分辨的分析工作流程。
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引用次数: 0
A multifunctional fluorescent sensing probe capable of sequential detection of trimethylamine and hydrogen sulfide produced by the spoilage of crabs and sole fish 一种多功能荧光传感探针,可连续检测螃蟹和比目鱼变质后产生的三甲胺和硫化氢
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-28 DOI: 10.1016/j.microc.2026.117110
Jiawen Liu , Shuo Yao , Changji Gao , Zhiwei Sun
In this work, we developed a fluorescent sensing probe named HTHB, capable of continuous detection of trimethylamine (TMA) and H2S, enabling phased monitoring of the freshness of crabs and sole fish. The probe HTHB inherently emits yellow fluorescence. Upon reaction with TMA, it shifts to emitting red fluorescence. Subsequently, exposure to H2S causes the fluorescence to change from red to blue. The fluorescence color changes significantly and the response speed is fast, with the entire continuous detection process completed within 1 min. Meanwhile, HTHB demonstrated high sensitivity and low detection limit for the two target substances. Subsequently, a detection hydrogel loaded with HTHB was prepared for the phased detection of the freshness of actual seafood. The results obtained by combining intelligent software color analysis and PCA analysis jointly verified the practical feasibility of this detection device. In addition, HTHB, with its fluorescence performance capable of achieving single detection of pH or H2S, can also be prepared into detection labels or detection solutions for real-time rapid detection of target substances in specific application environments. We believe that the probe HTHB has the potential to develop into an effective tool for staged freshness detection of crabs and sole fish, and promising applications in food quality monitoring and the research and development of fluorescent materials.
在这项工作中,我们开发了一种名为HTHB的荧光传感探针,可以连续检测三甲胺(TMA)和H2S,从而实现对螃蟹和比目鱼新鲜度的阶段性监测。探针HTHB本身发出黄色荧光。与TMA反应后,它转变为发出红色荧光。随后,暴露于H2S使荧光从红色变为蓝色。荧光颜色变化明显,响应速度快,整个连续检测过程在1 min内完成。同时,HTHB对两种目标物质的检测灵敏度高,检出限低。随后,制备了负载HTHB的检测水凝胶,用于实际海鲜新鲜度的阶段性检测。将智能软件色彩分析与PCA分析相结合得到的结果,共同验证了该检测装置的实际可行性。此外,HTHB的荧光性能可以实现pH或H2S的单次检测,也可以制备成检测标签或检测溶液,在特定的应用环境中对目标物质进行实时快速检测。我们认为HTHB探针有潜力发展成为螃蟹和比目鱼分阶段新鲜度检测的有效工具,在食品质量监测和荧光材料的研究与开发中具有广阔的应用前景。
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引用次数: 0
Washing away the fraud: Chemometric models for detecting falsified laundry detergent 洗去欺诈:检测伪造洗衣粉的化学计量模型
IF 4.9 2区 化学 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2026-01-28 DOI: 10.1016/j.microc.2026.117135
Ana Carolina da Costa Fulgêncio , Emanuel Felipe Souza Silva , Lucas Samuel Souza Almeida , Hélio Milito Martins de Amorim Neto , Rogério Araújo Lordeiro , Marcelo Martins Sena
It was observed a recent increase in the number of police occurrences seizing falsified laundry detergent in Brazil, in which the market leader brand has been counterfeited by replacing it with cheaper brands in fake packages. Thus, this article developed a direct and rapid screening analytical method based on portable near infrared (NIR) spectroscopy and chemometrics for checking the authenticity of samples of this leader brand of laundry detergent, aiming to detect counterfeiting. Supervised classification models were built with a total of 172 samples, including 83 certified authentic samples, 34 real counterfeit samples seized by the police, and 55 samples of cheaper brands used in these frauds. One-class modeling (soft independent modeling of class analogy, SIMCA, and data-driven SIMCA, DD-SIMCA) models were compared, and the best results were obtained with DD-SIMCA (no misclassification for the training set, false positive rate of 2.2% and false negative rate of 7.1% for the test set). Both methods were validated by estimating proper figures of merit and models were spectrally interpreted through the informative vector modeling power.
据观察,最近在巴西,警方查获假冒洗衣粉的案件有所增加,在这些案件中,市场领先品牌被假冒为更便宜的品牌,并装在假包装中。因此,本文开发了一种基于便携式近红外(NIR)光谱和化学计量学的直接快速筛选分析方法,用于检测该领导品牌洗衣液样品的真伪,旨在检测假冒产品。共建立了172个样品的监督分类模型,其中83个经过认证的正品样品,34个被警方查获的真品样品,以及55个用于这些欺诈的廉价品牌样品。单类建模(类类比的软独立建模,SIMCA和数据驱动的SIMCA, DD-SIMCA)模型进行比较,DD-SIMCA模型获得了最好的结果(训练集没有误分类,测试集的假阳性率为2.2%,假阴性率为7.1%)。两种方法都通过估计适当的优点值进行了验证,并通过信息向量建模能力对模型进行了频谱解释。
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引用次数: 0
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Microchemical Journal
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