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UHPLC-MS/MS
TALANTA · 2020 · IF 5.339

12-Plex UHPLC-MS/MS analysis of sarcosine in human urine using integrated principle of multiplex tags chemical isotope labeling and selective imprint enriching

Shi-En Chen,Jingwen Hu,Ping Yan,Jing Sun,Wenhui Jia,Shuyun Zhu,Xian-En Zhao,Huwei Liu

Urinary sarcosine was considered to be a potential biomarker for prostate cancer (Pca). In this work, an integrated strategy of multiplex tags chemical isotope labeling (MTCIL) combined with magnetic dispersive solid phase extraction (MDSPE), was proposed for specific extraction and high-throughput determination of sarcosine by ultra high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). In the past three months, we have developed 8-plex MTCIL reagents with excellent qualitative and quantitative performance. In this work, the multiplexing capacity of MTCIL reagents (MTCIL360/361/362/363/364/365/366/375/376/378/379/381) was increased 1.5-fold from 8-plex to 12-plex. MTCIL359 was prepared and used to label sarcosine standard as internal standard (IS). The structural analogue derivative (MTCIL373-sarcosine) of all targeted MTCIL-sarcosine derivatives was synthesized and used as a novel dummy template to prepare dummy magnetic molecularly imprinted polymers (DMMIPs). The integration of MTCIL and DMMIPs procedures were extremely favorable to excellent chromatographic separation and efficient mass spectrometric detection. The labeling efficiency, chromatographic retention and mass spectrometry responses of MTCIL reagents were consistent for sarcosine. In a single UHPLC-MS/MS run (2.0 min), this method can simultaneously quantify sarcosine in 12-plex urine samples and achieve unbiased concentrations comparison between different urine samples. Analytical parameters including linearity (R 2 0.989–0.997), detection limits (0.02 nM), precision (2.6–11.5%), accuracy (96.1–107.4%), matrix effect, labeling and extraction efficiency were carefully validated. The proposed method was successfully applied for urinary sarcosine determination of healthy male individuals and Pca patients. It was found that the sarcosine concentrations in these two groups were statistically extremely significantly different ( P  < 0.001). The developed method was a powerful analytical tool to substantially promote the analysis throughput and large-scale experiments about the potential biomarker research.

研究领域: 分析化学 · 医学 · 生物化学
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TALANTA · 2019 · IF 4.916

Graphene oxide-Fe3O4 nanocomposite magnetic solid phase extraction followed by UHPLC-MS/MS for highly sensitive determination of eight psychoactive drugs in urine samples

Qing Lu,Hao Guo,Yuanyuan Zhang,Xiaodong Tang,Weibin Lei,Ruijuan Qi,Junhao Chu,Dezeng Li,Qingbiao Zhao

Graphene oxide–Fe 3 O 4 (GO–Fe 3 O 4 ) nanocomposite was synthesized by a facile chemical co-precipitation method. The GO–Fe 3 O 4 was used as magnetic sorbent to extract the eight psychoactive drugs from urine samples. The analytes are morphine (MOR), 6-monoacetylmorphine (6-MAM), amphetamine (AMP), methamphetamine (MAMP), codeine, cocaine, dolantin and benzoylecgonine (BZE), which were determined by ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). This method has high selectivity for the target analytes. The limit of detection (LOD) and limit of quantification (LOQ) were 0.02–0.2 μg L −1 and 0.05–0.5 μg L −1 , respectively. The Mandel's fitting test revealed good linearity within all linear ranges. The linear ranges were calculated as 0.05–1000 μg L −1 for AMP, MAMP, cocaine and dolantin; 0.1–1000 μg L −1 for 6-MAM and codein; and 0.5–1000 μg L −1 for MOR and BZE. The recoveries ranged in 80.4–105.5%. The intra-day and inter-day RSDs are in the range of 2.7–13.1% and 3.9–13.7%, respectively. Magnetic solid phase extraction (MSPE) with GO–Fe 3 O 4 provides a convenient, rapid and green sample pretreatment method for extracting the target psychoactive drugs from urine. This methodology can be used for simultaneous or individual detection of eight major psychoactive drugs with high sensitivity. This method has high potential in clinical and forensic areas for psychoactive drugs analysis.

CAS / MDL: 1336-21-6 7783-85-9
研究领域: 分析化学 · 法医学 · 临床检验
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FOOD RESEARCH INTERNATIONAL · 2022 · IF 7.425

A novel UHPLC-MS/MS method for the determination of four α-dicarbonyl compounds in wine and dynamic monitoring in human urine after drinking

Chao Qi,Yueying Jin,Shengyu Cheng,Lei Di,Xin Wang,Minghui Zhang,Lingli Zhang,Xi-Ling Li,Yu Han,Qingkun Ma,Jun Zhe Min

α-dicarbonyl compounds (α-DCs) serve as potential biomarkers for oxidative stress-related diseases but are difficult to detect.   To study the metabolism of carbonyl compounds , we developed a new mass spectrometry probe, 3-benzyl-2-oxo-4λ 3 -thiazolidine-4-carbohydrazide (BOTC), containing hydrazyl groups for the targeted detection of carbonyl functional groups.   In a novel approach, we used BOTC pre-column derivatization with ultrahigh performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) to simultaneously detect four kinds of α-DCs in red wine as well as in urine after drinking. The α-DCs were completely separated (R 2  ≥ 0.9995), detection was sensitive (detection limit was 12.5–50 fmol), consistent (intraday and interday precision was 0.1–5.7 %), and efficient (average recoveries were 103.3–110.2 %). The method was applied to the analysis of α-DCs in different wines and the dynamic monitoring of transit and excretion in vivo after drinking. Our novel method provides a new strategy for the detection of α-dicarbonyl compounds in red wine and dicarbonyl compounds produced in oxidative stress-related diseases.

研究领域: 分析化学 · 医学 · 食品科学
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FOOD CHEMISTRY · 2024 · IF 8.5

Direct extraction of ten estrogens from milk samples with DVB/NVP-modified magnetic solid-phase extraction adsorbent followed by pre-column derivatization-UHPLC-MS/MS

Jiaxi Wen,Kehan Zhang,Yujun Liu,Zhifeng Du,Chaomei Xiong,Hongliang Jiang

Estrogens and their analogues can cause harm to human health through the food chain. Ten estrogens in different milk samples were directly extracted by amphiphilic divinylbenzene/ N -vinyl-2-pyrrolidone (DVB/NVP)-Fe 3 O 4 @SiO 2 -based magnetic solid-phase extraction (MSPE) followed by pre-column derivatization and ultra-high performance liquid chromatography tandem mass-spectrometry (UHPLC-MS/MS) detection. Under the optimal conditions, the limits of detection for ten analytes were in the range of 0.05–0.38 ng mL −1 in whole liquid milk matrix and 0.04–3.00 ng g −1 in milk powder matrix. The intra-/inter-day accuracy ranged in 83.4–113.8%, with RSDs in 2.5–15.0%. A total of 15 brands of liquid milk and milk powder samples were analyzed, and only estradiol was detected in three brands of boxed liquid milk within safe range. The proposed sample pretreatment eliminated the common protein precipitation process, improved the sample throughput, and has the potential for routine testing of estrogens and their analogues in market-sale milk samples.

CAS / MDL: 1321-74-0 10025-77-1
研究领域: 分析化学 · 食品安全 · 环境科学
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JOURNAL OF HAZARDOUS MATERIALS · 2020 · IF 9.038

Cationic metal-organic framework based mixed-matrix membrane for extraction of phenoxy carboxylic acid (PCA) herbicides from water samples followed by UHPLC-MS/MS determination

Gege Wu,Jiping Ma,Shasha Wang,Huining Chai,Liang Guo,Jinhua Li,Abbas Ostovan,Yafeng Guan,Lingxin Chen

A novel kind of cationic metal-organic framework(MOF) based mixed-matrix membrane(MMM) namely cationic MOF-MMM was firstly designed and used for simultaneous dispersive membrane extraction(DME) of six phenoxy carboxylic acid(PCA) herbicides from water samples followed by determination using ultrahigh-performance liquid chromatography tandem mass spectrometry. The cationic MOF-MMM was synthesized by soaking the zirconium-based MOFs in a polyvinylidene fluoride(PVDF) solution and further functionalization with quaternary amine groups, viz., UiO-66-NMe 3 + MMM. The well-prepared UiO-66-NMe 3 + MMM was characterized by FT-IR, SEM, XRD, XPS, NMR and etc. Several main variables influencing the MMM based DME efficiency were investigated and optimized in detail, such as dosage ratio of MOF/PVDF, solution pH, extraction time, coexistent anions and ionic strength. Electrostatic interactions dominated adsorption mechanism between anionic PCAs and cationic UiO-66-NMe 3 + MMM, along with π π conjugation and cation-π bonding, leading to better adsorption performance. Low limits of detection in the range of 0.03–0.59 ng/L and satisfactory recoveries within 80.06–117.40 % for all the PCAs are a reliable witness to demonstrate supreme sensitivity and the applicability of the developed method. By relying on the obtained results, the present work implied cationic MOF-MMM based DME can be a versatile and worthy utility for extraction of pollutants from different water samples with high throughput.

研究领域: 分析化学 · 环境科学
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ACS Food Science & Technology · 2025 · IF 2.8

Investigation on the Flavor Characterization of Edible Cooked Insect Clanis Bilineata Larva Products Using SPME-GC-TOF/MS, UHPLC-MS/MS Combined with Sensory Evaluation

Zhimei Fan,Danni Zhang,Xueqian Guo,Yiwen Zhu,Panpan Chen,Chenxi Qiu,Ninglong Zhang,Jian Zhang,Liqiong Niu,Xichang Wang,Yuan Liu

Clanis Bilineata larva (CBL) is a unique Chinese insect delicacy in Jiangsu Province, which is known for its umami taste and high protein nutrition. To develop its desired flavor, the quantitative descriptive analysis (QDA) combined with high throughput instruments were applied to analyze the sensory attributes and compounds of raw, boiled and roasted CBLs. Through QDA, cooked CBLs showed higher meaty odor intensities than Raw CBL significantly (p < 0.05). Compared with boiled CBL, the roasting process could generate the roasted meaty/beany odors and umami/savory taste while reducing the negative effects of grassy/boiled vegetable/earthy odors and bitter taste. Pearson correlation analyses results showed that meaty odor was highly correlated with compounds produced by fatty acid degradation such as hexanal and 1-octen-3-ol. Meanwhile, histidine was highly correlated with bitter and adenosine monophosphate was highly correlated with umami. The taste and odor of cooked CBLs are mainly formed from the lipid degradation, protein degradation and nucleotide degradation. This study provides insights to use a proper cooking process to develop consumer-friendly CBL products.

CAS / MDL: 67-56-1 75-05-8
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MICROCHEMICAL JOURNAL · 2026 · IF 5.2

Enhanced selective enrichment of hydroxylated polycyclic aromatic hydrocarbons from biological samples using 4-carboxy-3-fluorophenylboronic acid-functionalized magnetic sorbents with UHPLC-MS/MS detection

Yun Wu,Shuting Yang,Yanqun Yang,Lijuan Long,Shuixin Ding,Chunyan Su,Linchun Bao,Qianchun Zhang

A novel magnetic nanocomposite (FPB@PEI@PDA@Fe 3 O 4 ) was synthesized for selective enrichment of HPAHs. • The MSPE-UHPLC-MS/MS method was developed to quantify nine trace HPAHs in urine and serum. • The Langmuir model governs adsorption, involving π–π, hydrogen bonding, electrostatic, and boronate affinity interactions. Hydroxylated polycyclic aromatic hydrocarbons (HPAHs) are bioaccumulative and environmentally persistent contaminants, recognized for their significant carcinogenic potential. However, accurate analysis remains challenging due to the inherent complexity of biological matrices (e.g., high protein content and numerous interfering compounds) and the ultra-trace concentrations (ng/L or pg/L levels) at which HPAHs typically occur. The efficient isolation of these analytes therefore requires a specially designed sorbent capable of strong interactions with HPAHs. To address this challenge, we designed and synthesized a novel magnetic adsorbent, 4-carboxy-3-fluorophenylboronic acid-functionalized polyethylenimine-coated polydopamine@Fe 3 O 4 (FPB@PEI@PDA@Fe 3 O 4 ), for use in magnetic solid-phase extraction (MSPE). Leveraging the properties of this novel material, an efficient MSPE-ultra-high pressure liquid chromatography-mass spectrometry method was developed to isolate and quantify nine HPAHs in urine and serum, with high sensitivity and selectivity, a wide linear range (0.0050–10 μg/L), and low detection limits (1.5–40 ng/L). To validate its applicability for human biomonitoring, urine and serum samples were analyzed, and four HPAHs, 1-naphthol, 9-phenanthrol, 1-phenanthrol, and 4-phenanthrol, were identified and quantified. The method exhibited satisfactory accuracy and precision, with recoveries of 80.3%–114% and relative standard deviations of 2.4%–13%. These results enable further understanding of the distribution and potential risks of HPAHs, and the method facilitates more accurate human health assessment and environmental monitoring. Download: Download high-res image (135KB) Download: Download full-size image

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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2018 · IF 2.831

Determination of dexmedetomidine by UHPLC–MS/MS and its application to evaluate the effect of dexmedetomidine concentration on the target-controlled infusion concentration of propofol

Zhuoling Zheng,Shuyu Zhang,Wudi Ma,Lingyi Zhang,Ling Huang,Wenqi Huang,Min Huang,Zhongxing Wang,Jiali Li

The combination of dexmedetomidine (DEX) and propofol (PPF) is extensively used in the field of anaesthesiology. This study aimed to develop and validate a rapid, simple and sensitive ultra high-performance liquid chromatography-tandem mass spectrometry (UHPLC–MS/MS) method for the determination of DEX in human plasma. The method was applied to evaluate the effect of DEX concentration on the target-controlled infusion (TCI) concentration of PPF. Analytes were separated on a Waters XTERRA ® MS C18 column with a mobile phase of acetonitrile-methanol-water containing 0.1% formic acid and 5 mM ammonium acetate (70:10:20, v/v/v ) at a flow-rate of 0.3 mL/min. Mass spectrometry was performed in the positive selection reaction monitoring mode. The 201.12 → 95.12 and 515.29 → 275.68 mass transitions of DEX and IS (telmisartan), respectively, were monitored. The calibration curve of DEX was linear over the concentrations of 0.1–10 ng/mL. The intra-batch and inter-batch precisions of quality control samples were less than 10.05% and had accuracies of less than 6.25%. The newly developed method was successfully applied to quantify the DEX concentrations of plasma samples from 34 patients who were co-medicated with DEX prior to receiving anaesthesia by PPF. Results showed that comedication with DEX could reduce the requirements of PPF. Specifically, it was firstly found that the concentration of DEX is negatively correlated with the TCI concentration of PPF at the time of loss of consciousness.

CAS / MDL: 144701-48-4
研究领域: 药理学 · 麻醉学 · 临床医学
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EUROPEAN FOOD RESEARCH AND TECHNOLOGY · 2024 · IF 3

A novel UHPLC-MS/MS method for the determination of three selenoamino acids in organic selenium supplements and dynamic monitoring in human urine after consumption

Kong Xinxin,Zhang Lingli,Cai Ling,Cheng Shengyu,Li Xi-Ling,Jin Toufeng,Min Jun Zhe

Selenium (Se) is a vital trace element for mammals, but excessive intake can lead to selenium poisoning. To manage Se intake properly, this study developed a novel method using ultra-high performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS). This technique allows the simultaneous detection of three selenoamino acids in supplements. The three selenoamino acids were fully separated within 3 min. The method demonstrated excellent linearity (R 2  ≥ 0.9993), high sensitivity (detection limits were 2.49–2.92 fmol), and good precision (intraday and interday precision ranged from 2.87 to 13.54%). This study applied this method to analyze the content of selenoamino acids in organic selenium supplements from various sources and to dynamically monitor their absorption and excretion in the body after consumption. The novel approach offers a new strategy for the quality control of selenium-containing supplements and for studying selenium absorption and metabolism. Graphical abstract

CAS / MDL: 64-19-7 1464-42-2
研究领域: 分析化学 · 营养学 · 毒理学
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS · 2023 · IF 3.4

Study on herb-herb interaction between active components of Plantago asiatica L. seed and Coptis chinensis Franch. rhizoma based on transporters using UHPLC-MS/MS

Jieyu Zhang,Yan Chen,Wenxiang Fan,Linnan Li,Yueming Ma,Zhengtao Wang,Rong Shi,Li Yang

The combined efficacy in lowering serum lipid levels and increasing kidney protection of Plantago asiatica L. seed (Plantago) and Coptis chinensis Franch. rhizoma (Coptis) is far better than the effects of either herb alone. This finding suggests that there must be some degree of herb-herb interactions (HHI) affect potency. Here, we chose geniposidic acid (GPA), acteoside (ACT), and plantagoamidinic acid A (PLA) as active components in Plantago, and berberine (BBR) as the active component in Coptis, and, using transporter gene-transfected Madin-Darby canine kidney (MDCK) cells in combination with specific substrates and inhibitors, investigated Plantago- Coptis HHIs. We also established a UPLC-MS/MS analytical method to determine substrate content. Results showed that PLA in Plantago was a substrate of rOCT1/2 and rMATE1, and had inhibitory effects on rOCT2 and rMATE1. We also found that ACT is a substrate of rMATE1, but GPA was not a substrate of any transporter that we investigated. When BBR was used as the substrate, the inhibition rate of 10 μM PLA was 53.6% on rOCT2 and 31.5% on rMATE1. The inhibition rates of 30 μM ACT and 30 μM GPA on rMATE1 were 47.0% and 31.0%, respectively. Thus, our findings suggest that GPA, ACT, PLA, and BBR have competitive interactions that are driven by the rOCT2 and rMATE1 transporters. These interactions affect the transport and excretion of compounds and result in efficacy changes after co-administration.

CAS / MDL: 143664-11-3
研究领域: 药理学 · 药学 · 中药学 · 分析化学
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BIOMEDICAL CHROMATOGRAPHY · 2020 ·Vol. 34 ·期 8 ·e4845 · IF 1.728

Determination of plasma homocysteine with a UHPLC–MS/MS method: Application to analyze the correlation between plasma homocysteine and whole blood 5-methyltetrahydrofolate in healthy volunteers

Yubin Ji,Hongjun Luo,Hui Li,Zhexuan Lin,Wenhong Luo

An ultra-high performance liquid chromatography tandem mass spectrometry method was developed for determination of homocysteine (HCY) in human plasma. The HCY was derivatized with 2-chloro-1-methylquinolinium tetrafluoroborate and isolated using solid-phase extraction. Derivatization, isolation and detection procedures were optimized. Satisfactory linearity was obtained with determination coefficients ( r 2 ) >0.999. The intra- and inter-day precisions were in the interval of 1.2–5.1% and accuracy was within ±7%. Mean recoveries were close to 100%. The limit of detection and the limit of quantification were 0.46 and 1.38 μmol/L, respectively. The method was then applied to investigate the relationship between plasma HCY and whole blood 5-methyltetrahydrofolate levels in healthy volunteers. The results revealed that the plasma level of HCY was significantly negatively correlated to whole blood 5-methyltetrahydrofolate in volunteers.

研究领域: 医学检验 · 营养学
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MOLECULES · 2020 ·Vol. 25 ·期 4 ·897 · IF 3.267

NH2-MIL-53(Al) Polymer Monolithic Column for In-Tube Solid-Phase Microextraction Combined with UHPLC-MS/MS for Detection of Trace Sulfonamides in Food Samples

Qian-Chun Zhang,Guang-Ping Xia,Jun-Yi Liang,Xiao-Lan Zhang,Li Jiang,Yu-Guo Zheng,Xing-Yi Wang

In this study, a novel monolithic capillary column based on a NH2-MIL-53(Al) metal–organic framework (MOF) incorporated in poly (3-acrylamidophenylboronic acid/methacrylic acid-co-ethylene glycol dimethacrylate) (poly (AAPBA/MAA-co-EGDMA)) was prepared using an in situ polymerization method. The characteristics of the MOF-polymer monolithic column were investigated by scanning electron microscopy, Fourier-transform infrared spectroscopy, X-ray photoelectron spectroscopy, X-ray diffractometry, Brunauer-Emmett-Teller analysis, and thermogravimetric analysis. The prepared MOF-polymer monolithic column showed good permeability, high extraction efficiency, chemical stability, and good reproducibility. The MOF-polymer monolithic column was used for in-tube solid-phase microextraction (SPME) to efficiently adsorb trace sulfonamides from food samples. A novel method combining MOF-polymer-monolithic-column-based SPME with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was successfully developed. The linear range was from 0.015 to 25.0 µg/L, with low limits of detection of 1.3–4.7 ng/L and relative standard deviations (RSDs) of < 6.1%. Eight trace sulfonamides in fish and chicken samples were determined, with recoveries of the eight analytes ranging from 85.7% to 113% and acceptable RSDs of < 7.3%. These results demonstrate that the novel MOF-polymer-monolithic-column-based SPME coupled with UHPLC-MS/MS is a highly sensitive, practical, and convenient method for monitoring trace sulfonamides in food samples previously extracted with an adequate solvent.Keywords:monolithic capillary column;metal-organic framework;sulfonamides;solid-phase microextraction;ultra-high performance liquid chromatography-tandem mass spectrometry

CAS / MDL: 78-67-1
研究领域: 分析化学 · 食品科学 · 材料科学
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