Application of microcrystalline cellulose as an efficient and cheap sorbent for the extraction of metoprolol from plasma and wastewater before HPLC–MS/MS determination

A dispersive solid-phase extraction method based on a new sorbent has been performed on plasma and wastewater samples to determine metoprolol by high-performance liquid chromatography–tandem mass spectrometry. In this study, the analyte was adsorbed from the samples onto microcrystalline cellulose as a green and efficient sorbent and then eluted for use in the determination step. In the mass spectrometer, the analyte was detected in the positive mode and selectivity of the analysis was increased by sequential mass analysis through multiple reaction monitoring. All of the effective parameters in the extraction of metoprolol from plasma and wastewater were optimized. Under optimal conditions the method was linear in the ranges of 1–1,000 and 0.1–1,000 ng/ml in plasma and wastewater samples, respectively. The detection limits of the method were 0.30 and 0.03 ng/ml in plasma and wastewater samples, respectively. The data showed that the method provides low detection limit, wide linear range, good precision and high extraction recovery. Finally several plasma and wastewater samples were successfully analyzed using the method. The use of a small amount of a green and inexpensive sorbent and a low volume of plasma without the need for further pretreatment steps are the main advantages of the method.     

Development and validation of a liquid chromatography–tandem mass spectrometry method for the simultaneous analysis of androgens,estrogens, glucocorticoids and progestagens in human serum

We present a liquid chromatography tandem mass spectrometry method for the simultaneous analysis of 16 endogenous steroids (androgens, estrogens, glucocorticoids and progestogens) in human serum. Samples (250 μl of matrix) were extracted with t-butylmethyl ether prior to LC–MS/MS analysis. The chromatographic separation was achieved on a reversed-phase column using a methanol–water gradient. The HPLC was coupled to a triple quadrupole mass spectrometer equipped with an electrospray ionization source with acquisition in multiple reaction monitoring mode. The method was validated using surrogate matrices and human serum samples. The specificity of the method was confirmed for all of the considered steroids; linearity was also assessed (R² > 0.99, lack-of-fit test) in the ranges of concentrations investigated. The lower limits of quantification were in the range 10–400 pg/ml depending on the target steroid. Accuracy was in the range 85–115% for all target steroids except for the lower limit of quantitation levels where it was 80–120%. The extraction recovery was always >65%. No significant matrix effects were observed. To test the reliability of the method, the analysis of serum samples collected from 10 healthy subjects (5 M/5F) was performed. The present method can be used to identify the trajectories of deviation from the concentration normality ranges applied to disorders of the gonadal and adrenal axes.     

Construction and application of an electrochemical sensor based on graphene-MXene nanocomposites for baicalin detectionEI北大核心CSCD

Redox graphene-MXene(rGO-MXene) nanocomposites were prepared by ion polymerization and used to construct a highly sensitive electrochemical sensor for baicalin(BA) detection. The synergistic effect of rGO and MXene increased the specific surface area and electron transport capacity of the electrode, and significantly enhanced the electrochemical response of BA. The cyclic voltammetry and differential pulse voltammetry were used to investigate the electrochemical behavior of BA on the sensor. Under the optimal conditions, the peak current exhibited a good linear relationship with BA concentration in the range of 0. 05-10 μmol / L, and the limit of detection was as low as 28 nmol / L. The method was applied to analyze traditional Chinese medicine preparations containing baicalin, such as Qingkailing Capsule and Sanhuang Tablets with good accuracy and spiked recovery. The results were highly consistent with those of high performance liquid chromatography, providing a technical means for the rapid and sensitive detection of traditional Chinese medicine preparations. © 2022, Youke Publishing Co.,Ltd. All rights reserved.     

新型多孔材料用作色谱手性固定相

手性固定相是色谱法分离分析手性化合物的关键。近年来,随着材料科学的迅速发展,越来越多的新型手性材料被作为色谱固定相用于手性分离分析。本文综述了近5年来液相色谱、气相色谱和毛细管电色谱领域的新型手性固定相的研究进展,重点总结了基于手性多孔材料的新型手性固定相研究,最后对手性固定相的研究进行了总结与展望。     

Online large volume sample staking preconcentration and separation of enantiomeric GHRH analogs by capillary electrophoresis

A capillary electrophoresis method is proposed to analyze the four most well-known growth hormone–releasing hormone (GHRH) analogs that are misused by athletes. Dimethyl-β-cyclodextrin used as a chiral selector allowed, for the first time, the separation of those basic peptide analogs, including enantiopeptides (sermorelin and CJC-1293) that differ by the chirality of only one amino acid. To increase the method sensitivity, electrokinetic preconcentration methods have been investigated. The large volume sample stacking with polarity switching (PS-LVSS) method with an injected sample volume corresponding to 80% of the capillary one was found superior to the sweeping in terms of signal enhancement factor (SEF). Acid and organic solvent addition to the sample (0.1 mM phosphoric acid with 30% methanol) led to a twofold signal improvement, when compared to water as a matrix. We increased capillary dimensions to provide a signal enhancement through the injection of a larger sample volume. Finally, using a combination of the optimized PS-LVSS preconcentration with the chiral capillary zone electrophoresis (CZE), the GHRH analogs were separated and limits of detection between 75 and 200 ng/mL were reached. This method was successfully applied to urine after a desalting step. An optimized C18 SPE was used for that purpose in order to provide low sample conductivity (<130 µS/cm) and preserve the efficiency of LVSS preconcentration. SEF of 640 was obtained with desalted urine spiked with sermorelin by comparison to the CZE (without preconcentration) method.     

Determination of macrolides in livestock excreta by syringe purification coupled with liquid chromatography tandem mass spectrometryEI北大核心CSCD

A method of syringe-dispersive solid-phase extraction combined with ultrahigh performance liquid chromatography with tandem mass spectrometry for the simultanous determination of 10 macrolides in manurebased fertilizers was developed. After extraction with methanol and acetonitrile,the extracts were purified by insyringe dispersion solid-phase extraction in syringes pre-filled with 60 mg PSA and 30 mg C18. The resulted extracts were further separated by a BEH C18 column,detected by multiple reaction monitoring in electrospray positive ion mode,and quantified by matrix-matched external standard method. The results showed that the recoveries of the target compounds ranged from 70% to 110% at three spiked levels（10,30,and 50 μµg/kg）with the relative standard deviations ranged from 1.4% to 12%. The limits of detection and quantification were 0.57 1.75 and 2.77-5.40 μµg/kg,respectively. This method was suitable for the simultaneous determination of residual macrolides in organic fertilizers. © 2023, Youke Publishing Co.,Ltd. All rights reserved.     

凝胶渗透色谱-气相色谱-离子阱质谱法测定桔梗原药和当归提取物中101种农药残留

建立了凝胶渗透色谱（GPC）-气相色谱-离子阱质谱同时检测桔梗原药和当归提取物中101种农药残留的分析方法。方法采用乙腈超声辅助提取桔梗原药和当归提取物,浓缩提取液至近干后用乙酸乙酯-环己烷（1∶1, v/v）复溶,采用凝胶渗透色谱法（选取40 cm长、内径20 mm的凝胶渗透色谱柱）对样品进行净化,弃去前段含脂类、色素等杂质的流出液,收集17~30 min洗脱液并旋转蒸发浓缩至近干,甲苯1 mL定容上机。选用DB-5MS毛细管色谱柱分离待测物,通过离子阱质谱实现对101种农药残留的高效检测。方法通过优化前处理条件和离子阱二级质谱参数,有效降低了复杂中药基质对待测化合物的干扰,最大限度提高了样品中农药的定量准确性和回收率,101种农药3水平添加的平均回收率为58.3%~108.9%,每个添加水平10次独立重复测定的相对标准偏差为0.4%~16.5%,检出限（LOD）范围为0.2~40.0 μg/kg,可满足当前韩国、日本、欧洲规定的最大残留限量（maximum residue limits, MRLs）要求。方法具有操作简单快速、灵敏度高、重复性好等特点,凝胶渗透色谱技术的应用克服了固相萃取小柱净化容量不足的弊端,离子阱技术的应用可以进一步排除共流出基体杂质的干扰,提高定量和定性的准确性,检测效果优于常用的气相色谱-质谱法,是对中药中同时分析多种农药残留检测方法的有益补充。     

基于捕集柱阵列的制备型二维液相色谱纯化烟草中的4个组分

二维液相色谱(2D-LC)因具有较高的峰容量,在复杂样品的分离分析中获得了广泛的关注。然而,制备型2D-LC以纯化高纯单体为目标,在方法开发和设备构成等方面与分析型2D-LC有较大的不同,目前尚未得到充分的开发,在大规模的制备纯化中应用较少。本文以一套制备液相色谱模块为分离系统,以稀释泵、切换阀和捕集柱阵列为接口,构建了新型的制备型2D-LC系统,旨在规模化纯化多个活性成分。以烟叶中可以用作医药原料的烟碱、绿原酸、芦丁和茄尼醇等组分为目标物,考察了不同类型填料对样品的捕集效率、过载条件下的色谱保留行为等,优化了制备色谱条件。进而利用在线2D-LC系统实现了烟叶提取物的纯化,通过一次运行获得了4个高纯化合物。该系统具有中压色谱纯化成本低、系统在线运行自动化程度高、稳定性好及容易放大等优点。烟叶中活性化学成分的回收利用对促进烟草行业的发展及带动地方农业经济开发具有重大的意义。     

Cloud-Enabled Handheld NIR Spectroscopy: A Transformative Approach for Real-Time Forensic Analysis of Cannabis Specimens

In the past few years, there has been significant interest within the forensic community regarding the deployment of portable solutions that provide real-time results. This article introduces an innovative technology or technology architecture that enables the integration of a handheld device, specifically, Viavi MicroNIR, with a cloud-based system. This cloud system encompasses a server responsible for data processing and a mobile application acting as a user interface. To demonstrate the transformative impact of this technology on field operators, the analysis of cannabis specimens has been utilized. System's capacity to distinguish between CBD-type and THC-type cannabis has been particularly highlighted, along with the remarkable congruence observed between the near-infrared (NIR) spectra and the reference analytical method involving ultra-high-performance liquid chromatography (UHPLC) The article will present the advantages of this application primarily focusing on its potential to alleviate the burden on laboratories by expediting routine illicit drug analysis. Viavi MicroNIR technology provides laboratory personnel with additional time to handle more complex cases, thereby enhancing overall efficiency.     

An eco-friendly multi-analyte high-performance thin layer chromatographic densitometric determination of amoxicillin,metronidazole, and famotidine in their ternary mixtures and simulated gastric juice: A promising protocol for eradicating Helicobacter pylori

Gastrointestinal tract disorders constitute a heavy burden to healthcare providers. To eradicate Helicobacter pylori infection, different triple therapy protocols have been proposed. Among which are combinations of proton pump inhibitors (e.g., omeprazole), histamine-2 receptor antagonists (e.g., famotidine), along with antibiotics (e.g., amoxicillin). In this work, a sensitive and accurate high-performance thin-layer chromatographic method was developed for the simultaneous determination of amoxicillin, metronidazole, and famotidine in bulk powder and laboratory-prepared combined-tablet mixtures. Complete separation of the cited compounds was achieved using pre-coated silica gel plates with a mixture of methanol:chloroform:toluene:water:glacial acetic acid (5:2:1.5:0.5:0.1 v/v/v/v/v) as the mobile phase. The method was fully validated as per the international conference of harmonization guidelines. Good linearity, a correlation coefficient of 0.9991, was obtained in the concentration ranges 0.1–1.6 μg/band (amoxicillin), 0.1–0.9 μg/band (metronidazole), and 0.1–0.9 μg/band (famotidine). Since the method allowed the determination of the three compounds in combined tablets with a high degree of selectivity, accuracy, precision, with cost-effectiveness, it could be used for regular quality control. Moreover, the applicability of the proposed method was extended to the determination of the ternary mixture in simulated gastric juice. Method greenness was assessed using different green metrics.