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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2018 · IF 2.441

Microwave assisted extraction for the determination of chlorogenic acid in Flos Lonicerae by direct analysis in real time mass spectrometry (DART-MS)

Xiao-Hui Yao,Jian-Yi Xu,Jing-Yi Hao,Yi Wan,Tao Chen,Dong-Yang Zhang,Long Li

Flos Lonicerae was an important Chinese medicine. In this research, a microwave assisted extraction method was applied for the extraction of chlorogenic acid from Flos Lonicerae . The operating conditions were optimized using a Box–Behnken design test. Under the optimal conditions, the extraction yield of chlorogenic acid reached 32.52 ± 1.31 mg/g. Next, a direct analysis in real time mass spectrometry (DART-MS) method was utilized to quantify of chlorogenic acid in Flos Lonicerae extracts. The primary parameters were optimized to obtain maximum signal intensity. In the detection process of the actual samples, the results obtained by DART–MS are consistent with those obtained by HPLC method with short detection time and acceptable repeatability and precision (<15%). In addition, the DART–MS/MS method has several advantages, such as speed, low cost and simplicity. Therefore, the DART-MS method is an efficient method that can be applied in the quantification of chlorogenic acid in Flos Lonicerae.

研究领域: 中药学 · 分析化学
✓ 已验证 DOI PubMed 高影响因子
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Journal of Analysis and Testing · 2022 ·Vol. 7 ·期 2 ·163-171 · IF 0

A Modified QuEChERS-DART-MS/MS Technique for High-Throughput Detection of Organophosphate Nerve Agent Hydrolysis Products in Environmental Samples

Qu Gang,Chen Bo,Liu Shilei,Zhang Qiaoli,Yang Yang,Fu Qingshan

Organophosphate nerve agents (OPNAs) are lethal chemical weapons (CWs) which hydrolyze rapidly to alkyl phosphate compounds in the environment. The identification of alkyl phosphate compounds in the environment is critical for the verification of OPNAs. Currently, due to the complex sample preparation and long detection process for organophosphate nerve agent hydrolysis products (OPNAHPs), their high-throughput determination is difficult. To simplify sample preparation and detection of OPNAHPs from environmental samples, a quick, easy, cheap, effective, rugged and safe (QuEChERS) method for the simultaneous purification of the five OPNAHPs in environmental samples combined with detection through direct analysis in real-time ionization source coupled with tandem mass spectrometer (DART-MS/MS) was developed. An internal standard method was applied for the quantification. The method exhibited a good linearity ( R 2  > 0.991) in the range of 1.00 ng/mL-4.00 μg/mL. The limits of detection and limits of quantification were 1.00–7.00 ng/mL and 10.0–20.0 ng/mL, respectively. The recoveries of OPNAHPs in environmental samples were between 65.3% and 107%, with relative standard deviations ranged from 1.6% to 19%. In addition, the sample preparation and analysis process for OPNAHPs could be completed in less than 10 min. The results demonstrated that the modified QuEChERS method could quickly and efficiently remove the matrix of environmental samples. Combined with DART-MS/MS, an accurate and high-throughput detection method of OPNAHPs in environmental samples was provided. The developed method has great potential in the fields of early warning, clinical treatment and environmental decontamination.

CAS / MDL: 18623-11-5
研究领域: 分析化学 · 环境科学 · 毒理学
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ANALYTICA CHIMICA ACTA · 2013 · IF 4.387

On-line coupling of macroporous resin column chromatography with direct analysis in real time mass spectrometry utilizing a surface flowing mode sample holder

Shanshan Zeng,Lu Wang,Teng Chen,Haibin Qu

A surface flowing mode sample holder was designed as an alternative sampling strategy for direct analysis in real time mass spectrometry (DART-MS). With the sample holder, the on-line coupling of macroporous resin column chromatography with DART-MS was explored and the new system was employed to monitor the column chromatography elution process of Panax notoginseng . The effluent from macroporous resin column was first diluted and mixed with a derivatization reagent on-line, and the mixture was then directly transferred into the ionization region of DART-MS by the sample holder. Notoginsenosides were methylated and ionized in a metastable helium gas stream , and was introduced into MS for detection. The on-line system showed reasonable repeatability with a relative standard deviation of 12.3% for the peak area. Three notoginsenosides, i.e. notoginsenoside R 1 , ginsenoside Rb 1 and ginsenoside Rg 1 , were simultaneously determined during the eluting process. The alteration of the chemical composition in the effluent was accurately identified in 9   min, agreeing well with the off-line analysis. The presented technique is more convenient compared to the traditional UPLC method. These results suggest that the surface flowing mode DART-MS has a good potential for the on-line process monitoring in the pharmaceutical industry .

CAS / MDL: 75-59-2
研究领域: 分析化学 · 中药学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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MOLECULES · 2023 ·Vol. 28 ·期 10 ·4131 · IF 4.6

The Study of Alanine Transaminase Activity in Tissues of Silkworm (Bombyx mori) via Direct Analysis in Real-Time (DART) Mass Spectrometry

Guohua Wu,Lei Jiang,Jianjun Guo,Wushuang Li,Lin Ma,Bozhi Tang,Charles C. Liu

Alanine transaminase (ALT) is an important amino acid-metabolizing enzyme in silkwormBombyx moriL., and is mainly involved in transferring glutamate to alanine (serving as an essential precursor in silk protein synthesis) through transamination. Therefore, it is generally believed that silk protein synthesis in the silk gland and the cocoon quantity increase with the increase in ALT activity to a certain extent. Here, a novel analytical method was developed to determine the ALT activity in several key tissues ofBombyx moriL. including the posterior silk gland, midgut, fat body, middle silk gland, trachea and hemolymph, by combining the direct-analysis-in-real-time (DART) ion source with a triple-quadrupole mass spectrometer. In addition, a traditional ALT activity assay, the Reitman–Frankel method, was also used to measure ALT activity for comparison. The ALT activity results obtained via the DART-MS method are in good agreement with those obtained via the Reitman–Frankel method. However, the present DART-MS method provides a more convenient, rapid and environmentally friendly quantitative method for ALT measurement. Especially, this method can also monitor ALT activity in different tissues ofBombyx moriL. in real time.Keywords:ALT;DART-MS;Bombyx mori;biochemical analysis

研究领域: 昆虫学 · 生物化学
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NEW JOURNAL OF CHEMISTRY · 2016 ·Vol. 41 ·期 3 ·1103-1109 · IF 3.277

Ionization characteristics of glycosides by direct analysis in real time quadrupole-time of flight mass spectrometry

Hongmei Yang,Ge Gao,Yihan Wang,Jinrong Liu,Zongjun Li,Rui Su,Bing Wang,Wenhui Lian,Xinhua Guo,Shuying Liu

Glycosides, which are widely distributed in many plants, possess numerous biological activities. Direct analysis in real time (DART) allows the rapid analysis of samples or objects in their native state in the open environment. The ionization characteristics of glycosides by DART, however, have not yet been investigated in detail. DART quadrupole-time of flight mass spectrometry (DART-Q-TOF-MS) was developed to investigate the ionization characteristics of different kinds of glycosides in both positive and negative ion modes. All the glycosides were ionized via various different reactions including (de)protonation, molecular ion formation, ISD fragmentation, and the formation of adducts. In contrast, glycosidic cleavage ions and molecular ions (radical ions) were easily detected in negative DART mass spectra by the capture of an electron. The degree of glycosidic cleavage varied with the structural properties of individual glycosides, which were substantiated by theoretical calculations using the software package Gaussian 09. Temperature and types of DART gas played important roles in DART mass spectrometric analysis of glycosides.

研究领域: 分析化学 · 植物化学
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ANALYTICAL CHEMISTRY · 2018 · IF 6.042

Direct Analysis in Real Time Mass Spectrometry for Characterization of Large Saccharides

Huiying Ma,Qing Jiang,Diya Dai,Hongli Li,Wentao Bi,David Da Yong Chen

Polysaccharide characterization posts the most difficult challenge to available analytical technologies compared to other types of biomolecules. Plant polysaccharides are reported to have numerous medicinal values, but their effect can be different based on the types of plants, and even regions of productions and conditions of cultivation. However, the molecular basis of the differences of these polysaccharides is largely unknown. In this study, direct analysis in real time mass spectrometry (DART-MS) was used to generate polysaccharide fingerprints. Large saccharides can break down into characteristic small fragments in the DART source via pyrolysis, and the products are then detected by high resolution MS. Temperature was shown to be a crucial parameter for the decomposition of large polysaccharide. The general behavior of carbohydrates in DART-MS was also studied through the investigation of a number of mono- and oligosaccharide standards. The chemical formula and putative ionic forms of the fragments were proposed based on accurate mass with less than 10 ppm mass errors. Multivariate data analysis shows the clear differentiation of different plant species. Intensities of marker ions compared among samples also showed obvious differences. The combination of DART-MS analysis and mechanochemical extraction method used in this work demonstrates a simple, fast, and high throughput analytical protocol for the efficient evaluation of molecular features in plant polysaccharides.

研究领域: 分析化学 · 植物学 · 药理学
✓ 已验证 DOI PubMed 高影响因子
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY · 2023 ·Vol. 415 ·期 18 ·4343-4352 · IF 4.3

Influence of host–guest interactions on analytical performance of direct analysis in real-time mass spectrometry

Liu Min,Wang Simin,Ge Wuxia,Bi Wentao,Chen David Da Yong

To systematically study the influence of host–guest interactions on the analytical performance of direct analysis in real time mass spectrometry (DART-MS), the interactions between cyclodextrins (CDs) and different Sudan dyes were investigated. The results showed that the host–guest interaction between CDs and Sudan dyes did not affect qualitative analysis of the target compounds, but led to a lower signal intensity for Sudan dyes, thus affecting quantitative analysis of the target compounds. The stronger the host–guest interaction, the weaker the signal intensity of target compound on DART-MS. The results also show that both in solution and in solid-phase microextraction (SPME), the addition of organic solvents can weaken the host–guest interaction between CDs and Sudan dyes, thus improving the signal intensity in DART-MS. In SPME, adding organic solvents has a certain practical value and can improve the efficiency of Sudan dye analysis. This study suggests that appropriate sample pretreatment is needed to weaken noncovalent interactions prior to DART-MS analysis to obtain more accurate quantitative results. The data provide some insight into the effects of other noncovalent interactions on the efficiency of DART-MS as an analytical tool, as well as the potential to study intermolecular interactions with DART-MS. Graphical Abstract

研究领域: 分析化学 · 质谱分析
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TALANTA · 2019 · IF 4.916

Nanofibers mat as sampling module of direct analysis in real time mass spectrometry for sensitive and high-throughput screening of illegally adulterated sulfonylureas in antidiabetic health-care teas

Jiankun Cao,Qing Jiang,Ruixian Li,Qian Xu,Hongli Li

In this work, novel ionic liquid (IL) functionalized polyacrylonitrile nanofibers mat (IL/PAN–NFsM) was firstly prepared through thiol–ene “click” reaction and evaluated for the establishment of a sensitive and high-throughput screening method. Because of its excellent pre-separation efficiency, IL/PAN–NFsM can adsorb trace-level targets from complex sample matrix within tens of seconds by performing a solid-phase extraction (SPE) process, and then served as sampling modules of direct analysis real time mass spectrometry (DART–MS) without any additional processing. This means the target analytes concentrated on IL/PAN–NFsM were directly desorbed, ionized, and detected by DART–MS. To verify the feasibility of the proposed method, three illegal added synthetic drugs (gliclazide, glimepiride , and gliquidone) were screened in six types of antidiabetic health-care tea samples. The results indicated that the sensitivity is in the level of ng g −1 , while total analysis time does not exceed 1.0 min per sample. Moreover, the stability expressed as relative standard deviation (RSD) varies from 1.7% to 17.3%. We proposed a new screening mode based on the direct combination of functionalized NFsM and DART–MS, which is expected to become a universal method in food safety analysis.

研究领域: 分析化学 · 食品安全 · 药物分析
✓ 已验证 产品关联 DOI PubMed 高影响因子
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TALANTA · 2026 · IF 6.7

Stereoselective cyclic peptide assisted DART-MS for rapidly screening environmental disruptors of dopamine receptors

Yiheng Yuan,Hongyu Wen,Geng Li,Yong Shen,Ling Fang,Jianqiao Xu,Gangfeng Ouyang

The emerging binding-directed analysis (BDA) technique has successfully employed stereoselective oligopeptide probes to capture G protein-coupled receptor (GPCR)-active compounds from complex environmental matrices via electrospray ionization (ESI)-enabled complex formation. However, its integration with direct analysis in real time-mass spectrometry (DART-MS), a technique characterized by fundamentally different ionization mechanisms and exceptionally high analytical throughput, remains unexplored. This study evaluates a DART-MS-based BDA workflow for rapid, chromatography-free screening of GPCR ligands using ten model dopamine (DA) receptor ligands and a dopamine-selective cyclic peptide probe (CPP). The workflow required less than 1 min per measurement. Notably, DART-MS even achieved an average CPP-ligand complexation efficiency substantially higher than that obtained in ESI-MS (20% vs 4%), facilitating reliable identification of CPP-ligand complex ions from redundant mass spectra. Moreover, most CPP-ligand gas-phase complexes formed in DART-MS and ESI-MS showed comparable collision stability. Only the CPP-sulpiride and CPP-pramipexole complexes showed stability reduction by 85% and 61% in DART-MS compared to ESI-MS. These findings suggest that DART desorption/ionization conditions may promote more efficient formation and/or preservation of CPP-ligand complex ions. The applicability of the DART-MS-based BDA workflow was further validated through analysis of surface water samples. Although the spiked model ligand perphenazine (L1) was not captured by the CPP, the rubber additive 1,3-diphenylguanidine was successfully identified, a DA antagonist formerly also discovered by the ESI-MS-based BDA workflow. Collectively, this study establishes DART-MS-based BDA as a highly-efficient screening tool for future large-scale surveillance of GPCR-disrupting chemicals in the environment.

✓ 已验证 DOI PubMed 高影响因子
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ANALYTICAL CHEMISTRY · 2021 · IF 6.986

Tee-Shaped Sample Introduction Device Coupled with Direct Analysis in Real-Time Mass Spectrometry for Gaseous Analytes

Xin Geng,Zhengyan Zhao,Hongli Li,David Da Yong Chen

Ambient ionization mass spectrometry (AIMS) is simple to operate for analytes adsorbed on the surface of various shaped probes. However, gaseous substances or liquids that are easy to evaporate, diffuse, and escape in the atmosphere are harder to capture. In this work, a Tee-shaped sample introduction device coupled with direct analysis in real time mass spectrometry (DART-MS) is developed. The Tee-shaped device is placed between the DART ion source and the MS inlet with a heated sample transfer tube. Gaseous samples from either a Tedlar sampling bag or liquids evaporated from a graduated syringe were tested. The Tee-shaped device was used for several volatile organic compounds with a wide range of boiling points, and detection limits of ng/mL to fg/mL were obtained. To test the device for real-life samples, puff-by-puff analysis of a complex gaseous mainstream smoke was performed. Individual puffs can be analyzed rapidly, and there is no cross contamination between consecutive puffs. The dynamic changes of chemical components among different puffs for different types of cigarettes can be observed. This work provides a universal Tee-shaped sampling device to enhance AIMS for the analysis of volatile compounds and gases, which is adapted to different sampling modules applicable for various forms of samples. The device enables direct exploration of chemical components in complex gaseous samples without tedious sample preparation and time-consuming LC or GC separation.

研究领域: 分析化学 · 环境科学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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ANALYTICAL AND BIOANALYTICAL CHEMISTRY · 2025 · IF 3.8

High-throughput quantification of butachlor by DART-MS/MS coupled with micro-solid-phase extraction and dual fragmentation to enhance selectivity and sensitivity

Li Huaqiang,Wu Feifei,Ding Yuxian,Long Guozhou,Yin Lei

A novel and rapid analytical assay based on direct analysis in real-time tandem mass spectrometry (DART-MS/MS) technology was established for quantification of butachlor in this study. The assay incorporated micro-solid-phase extraction (μ-SPE) for sample pretreatment, with acetochlor as an internal standard. Quantification was achieved via transitions from [M + H] + precursor ions to primary and secondary fragment ions at m/z 312.1 → 238.0 → 162.1 (butachlor) and 270.1 → 224.1 → 148.0 (acetochlor). This chromatography-free approach eliminated reliance on mobile phases and chromatographic instrumentation, significantly improving analytical throughput (0.4 min/sample) while reducing environmental impact. Method validation demonstrated linearity over 0.5–100 ng/mL ( R 2  > 0.995), with intra-/inter-day precision < 13.1% and accuracy ranging from −6.00% to 11.0%. The assay was used to evaluate the cellular uptake kinetics of butachlor in MCF-7 cells. These findings underscore the utility of DART-MS/MS assay for rapid environmental and toxicological assessments while highlighting potential safety concerns associated with butachlor exposure. The integration of DART-MS/MS with μ-SPE offers a sustainable alternative to conventional bioanalytical workflows, combining speed, sensitivity, and reduced chemical consumption for ecotoxicological studies. Graphical abstract

CAS / MDL: 23184-66-9 34256-82-1
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