MOLECULES
·
2020
·Vol. 25
·期 4
·839
·
IF 3.267
Yueqing Xu,Liangxiao Zhang,Ruinan Yang,Xu Yu,Li Yu,Fei Ma,Hui Li,Xiupin Wang,Peiwu Li
Vitamin K1is one of the important hydrophobic vitamins in fat-containing foods. Traditionally, lipase is employed in the determination of vitamin K1to remove the lipids, which makes the detection complex, time-consuming, and insensitive. In this study, the determination of vitamin K1in fat-containing foods was developed based on ultrasound-assisted extraction (UAE), solid-phase extraction (SPE) combined with liquid chromatography–tandem mass spectrometry (LC-MS/MS). The optimal conditions for extraction of vitamin K1were material–liquid ratio of 1:70 (g/mL), extraction temperature of 50 °C, extraction power of 700 W, extraction time of 50 min, material-wash fluid ratio of 1:60 (g/mL), and 8 mL of hexane/anhydrous ether (97:3,v/v) as the elution solvent. Then, vitamin K1was analyzed on a ZORBAX SB-C18 column (50 mm × 2.1 mm, 1.8 μm) by gradient elution with water (0.01% formic acid) and methanol (0.01 formic acid + 2.5 mmol/L ammonium formate) as the mobile phase. The limit of detection (LOD) and limit of quantification (LOQ) were 0.05 and 0.16 μg/kg, respectively. Calibration curve was linear over the range of 10–500 ng/mL (R2> 0.9988). The recoveries at three spiked levels were between 80.9% and 119.1%. The validation and application indicated that the proposed method was simple and sensitive in determination of vitamin K1in fat-containing foods.Keywords:ultrasound-assisted extraction;solid-phase extraction;LC-MS/MS;vitamin K1;foods
研究领域:
分析化学
·
营养学
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DOI
PubMed
高影响因子
Water
·
2022
·Vol. 14
·期 15
·2371
·
IF 3.53
Huili Tang,Ziru Li,Hanqing Chen,Yang Xu,Xu Jiang,Erdeng Du,Zhen Lyu,Lu Zheng,Mingguo Peng
N-nitrosamines have recently attracted attention as a class of disinfection byproducts and are also a hot spot in environmental studies. Current N-nitrosamine analytical methods typically involve manual solid phase extraction (SPE) of samples followed by quantitative analysis using liquid chromatography-mass spectrometry (LCMS), which is time-consuming and may also fail to eliminate complex matrix effects. Size exclusion chromatography (SEC) is a technique that can separate compounds according to their molecular size. For the first time, this study developed an Online-SPE/SEC/LCMS quantitative analysis method to detect and analyze nine common N-nitrosamine disinfection byproducts in wastewater plant tailwater, including N-dimethylnitrosamine (NDMA) and N-nitrosodiethylamine (NDEA), etc. The samples of 1.0 mL can be directly injected after the simple 0.22 μm membrane filtration. This method reports the combination of SPE, SEC, and RP C18 columns to achieve several functions in a processing time of 20 min, including online enrichment, desalination, and matrix separation for the first time. The method provides good linearity (R2> 0.999), recoveries ranging from 91.67% to 105.88%, relative standard deviation (RSD) lower than 4.17%, and the limits of detection (LOD) are 0.12–6.60 ng/L. This method alleviates tedious human labor and can effectively overcome the matrix effect (ME< 20%). This method allows for the accurate quantitative analysis of N-nitrosamines with high compatibility in wastewater plant tailwater, rivers, and lakes with a high background matrix. Interested researchers can also use this method as a reference in the online analysis of other specific pollutants after necessary optimization. It can also be utilized for non-targeted screening and targeted analysis of contaminants in water with a wide range of applications, giving valuable information for environmental monitoring.Keywords:N-nitrosamines;analysis method;online solid-phase extraction (Online-SPE);size exclusion chromatography (SEC);LCMS;column switching;wastewater plant tailwater
研究领域:
环境科学
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分析化学
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DOI
高影响因子
Analytical Methods
·
2025
·
IF 2.6
Rongting Zhuo,Rong Bao,Yanzhong Fan,Qi Lin,yan yang
Residues of pharmaceuticals and personal care products (PPCPs) in drinking water pose significant public health risks. To assess these residues in water, this study developed a solid-phase extraction combined with ultra-performance liquid chromatography-tandem mass spectrometry method (SPE-UPLC-MS/MS) for the simultaneous quantitative determination of 98 PPCP residues in drinking water. By optimizing the pretreatment method and analysis conditions, the method exhibits excellent linearity, with all PPCPs showing correlation coefficients (R²) greater than 0.99 within the concentration range of 0-100 μg/L. Recovery rates ranged from 60.7% to 119.0%, and the relative standard deviations (RSDs) below 20%. The limits of detection (LODs) were between 0.034 and 4.001 ng/L. Residues such as amisupride and 1,7-dimethylxanthine were detected in water samples. This method is simple, sensitive, and suitable for high-throughput detection of trace PPCPs in drinking water, providing reliable technical support for water quality monitoring.
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
International Journal of Electrochemical Science
·
2023
·Vol. 13
·期 7
·7129-7140
·
IF 1.5
Weigang Wu,Caiyan Liu,Fang Huang,Huaying Li,Yuting Wang,Ding Hong,Shi Wang,Xiaobin Zeng
In this work, a simple and novel method for determination of brain serotonin (5-HT) in depression mice was proposed with modified screen-printed electrode based on MWNTs/Al 2 O 3 /chitosan. The modified SPE displayed excellent electrocatalytic activity towards the oxidation of 5-HT in real brain tissue samples. Square wave voltammetry (SWV) was employed to optimize the experimental conditions. The proposed sensor showed voltammetric responses with high and good sensitivity for 5-HT in optimal conditions. The peak current of 5-HT was proportional to the concentration in the range of 0.01 μM to 1.0 μM with the detection limit 0.005 μM. Compared with the HPLC method, the newly developed method also presented good results in the detection of brain 5-HT level, which made it possible for helping depression desiease diagnosis. In conlusion, our experimental results strongly suggested that the established SPE could be used to the fast depression determination of 5-HT, which might offer a potential minotor tool for in future.
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DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
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2013
·
IF 2.591
Xiaoji Cao,Jiaoyu Chen,Xuemin Ye,Feifei Zhang,Lingxiao Shen,Weimin Mo
An ultrasound-assisted magnetic SPE procedure with an Fe 3 O 4 -grafted graphene nanocomposite as the magnetic adsorbent has been developed to determine seven polychlorinated biphenyls (PCBs; PCB28, PCB52, PCB101, PCB118, PCB138, PCB153, and PCB180) simultaneously in 200 mL environmental water samples, in combination with GC–MS/MS. Several factors related to magnetic SPE efficiencies, such as the superparamagnetic intensity and amount of adsorbent, extraction time, sample pH, and desorption conditions were investigated. With the assistance of ultrasound, the extraction achieved the maximum within only 20 s, attributed to the powerful adsorptive ability of the magnetic adsorbent toward the PCBs. Under the optimized conditions, an excellent linearity was observed in the range of 0.1–100 ng/L for PCB28, 0.2–100 ng/L for PCB52, and 0.5–100 ng/L for the other five PCBs with the correlation coefficients ranging from 0.9988 to 0.9996. The mean recoveries at spiked levels of 5.0 and 10.0 ng/L were 84.9–108.5%, the coefficients of variations were <6.5%. With convenient magnetic separation, the synthesized magnetic adsorbent could be recycled more than ten times. The proposed method was demonstrated to be feasible, simple, rapid, and easy to operate for the trace analysis of the PCBs in environmental water samples.
研究领域:
环境科学
·
分析化学
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产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2018
·
IF 2.746
Junlei He,Jiahao Yuan,Juan Du,Xiaoguang Chen,Xinguo Zhang,Ande Ma,Jialiang Pan
An automated on-line solid-phase extraction (SPE) method coupled with high performance liquid chromatography (HPLC) was developed for the first application to rapid quantification of trace amisulpride in human plasma. A kind of restricted-access media (RAM) column (Capcell Pak MF Ph-1) was adopted for highly efficient extraction of amisulpride and meanwhile for the limited access of macromolecular matrices. It was robust and reusable for >1000 times. The utilization of two programmable pumps enabled the simultaneous execution of SPE and HPLC analysis within 10 min. Additionally, using appropriate valve-switching time was found to efficiently reduce the contamination of HPLC system caused by co-elution of impurity from an RAM column, facilitating continuous analysis of large-scale samples. The method was characterized by free of internal standard (IS), which exhibited low limit of detection (0.0035 μg·mL −1 ), satisfactory precision and accuracy (recoveries of 98.1%–104.6% with relative standard deviations below 4.6%). Amisulpride was successfully detected in the plasma samples originated from four patients. Notably, interindividual differences of plasma sample matrices did not yield an adverse effect on the accuracy of our IS-free method. The comparison to previous methods shows the superiority of the method in terms of sensitivity, IS requirement, speed, and automation. Thus, the method has great potential for the application to therapeutic drug monitoring as well as large-scale bioanalytical and clinical studies.
研究领域:
分析化学
·
临床医学
·
药物分析
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DOI
高影响因子
Food Analytical Methods
·
2023
·Vol. 16
·期 4
·689-698
·
IF 2.9
Chu Qiqi,Wu Xinze,Chen Huaixia,Dang Xueping,Liu Xiaolan
A Cu 7 Zn 2 cluster functionalized copolymer monolithic column was prepared and applied as the adsorbent of pipette tip micro-solid phase microextraction of eight phthalate esters (PAEs). The physical morphology, chemical composition, thermal stability, and specific surface area of the monolithic column were characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy, thermogravimetric analysis, and N 2 adsorption and desorption experiment. Cu 7 Zn 2 cluster acted as the adsorption site effectively improved the adsorption selectivity and capacity of the copolymer monolith for PAEs. The adsorption mechanism of Cu 7 Zn 2 copolymer monolith for 8 PAEs was deduced to be mainly the H-bond interaction. And, the chemical doping and copolymerization of Cu 7 Zn 2 cluster made the composite monolithic column more stable with a long service life. Under the optimized extraction conditions, a micro-solid phase extraction-high performance liquid chromatography method with ultraviolet detector (μ-SPE-HPLC-UV) was developed for the determination of 8 PAEs in edible oil. Wide linear ranges of 0.5–1000 μg/kg with correlation coefficients ( R 2 ) above 0.996 were obtained. The limits of detection (LODs) were in the range of 0.1–0.9 μg/kg. The proposed method was applied for the detection of 8 PAEs in edible oil with satisfactory recoveries between 83.5~100.2%, and the relative standard deviations were less than 8.1%. The results indicated that the Cu 7 Zn 2 functionalized copolymerized monolithic column was an ideal enrichment medium for the detection of PAEs in complex samples.
研究领域:
分析化学
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环境科学
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材料科学
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DOI
高影响因子
CHROMATOGRAPHIA
·
2014
·Vol. 77
·期 23
·1705-1712
·
IF 1.37
Zhaoling Jiang,Lifang Zhang,Chong Zhang,Xiao Zhang,Feiqun Xue
Ultra high performance liquid chromatography with UV detection was developed and validated for the simultaneous determination of residues of toltrazuril and its two metabolites, namely, toltrazuril sulphone and toltrazuril sulphoxide, in edible tissues (chicken and porcine muscle, liver and kidney). Acetonitrile was used to extract analytes from tissues, which were then cleaned using primary secondary amine and Oasis™ MAX solid phase extraction cartridges. Chromatographic separation was performed on a C 18 column with gradient elution. The analytes were determined using a UV detector. The regression coefficients of matrix-matched calibration curves showed linearity of >0.99. Calibration ranged from 25 to 1,000 μg kg −1 for toltrazuril and toltrazuril sulphone, and 37.5–1,500 μg kg −1 for toltrazuril sulphoxide. The accuracy was between 80 and 110 %, and the inter and intraday RSDs were lower than 15.2 and 18.3 %, respectively. The limits of detection for toltrazuril, toltrazuril sulphone and toltrazuril sulphoxide were between 10 and 37.5 μg kg −1 in all the tissues. The developed method was successfully applied to detect toltrazuril, toltrazuril sulphone and toltrazuril sulphoxide in tissues of medicated chicken.
研究领域:
分析化学
·
兽医学
·
食品科学
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DOI
高影响因子
FOOD CHEMISTRY
·
2026
·
IF 10.4
Xinrui Yang,Xiaoling Chen,Gaohan Li,Yang Zhou,Qinhua Chen,Jinjun Hou,Changwu Zheng,Zijia Zhang,Wanying Wu
Areca nut ( Areca catechu L.) is a widely consumed food and medicinal plant with both nutritional value and documented health risks. To comprehensively characterize its chemical composition and spatial distribution, we developed an integrated analytical platform combining solid-phase extraction (SPE), offline two-dimensional liquid chromatography with high-resolution mass spectrometry (2D-LC-HRMS), and desorption electrospray ionization mass spectrometry imaging (DESI-MSI). This approach enriched trace constituents while minimizing matrix interference, enabling the identification of 323 compounds-including terpenes and triterpenoids (89), alkaloids (52), flavonoids (31), lignans (17), and steroids (12). A pH-orthogonal separation system (alkaline and acidic modes) significantly improved resolution of structurally similar, low-abundance compounds. Spatial analysis via DESI-MSI revealed three distribution patterns: seed-specific enrichment, pericarp enrichment, and uniform distribution. By integrating compositional and spatial data, this study offers new insights into the pharmacological basis, potential toxicity mechanisms, and safe applications of areca nut in food systems.
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DOI
PubMed
高影响因子
Sustainable Chemistry and Pharmacy
·
2025
·
IF 5.8
Ting Zhang,Danni Ma,Jiaxing Gong,Bolun Sun,Fuman Cai
Rare earth elements are essential components in renewable energy technologies and advanced functional materials. Despite their critical importance, they are typically present in low concentrations and are in increasingly high demand. Current mining and refining processes are energy intensive and cause significant environmental pollution. Therefore, there is an urgent need for eco-friendly, rapid, and effective analytical methods for their exploration. Traditional detection techniques are often costly, time-consuming, and non-portable. There remains a critical gap in the availability of rapid, sensitive, and economical sensors for rare earth element detection. In this study, we introduce a novel portable electrochemical detection system. This system utilizes a recombinant plasmid constructed using a codon-optimized gene to heterologously express a high-affinity protein that binds rare-earth ions. It integrates a graphene oxide-coated screen-printed electrode with an electrochemical workstation for the detection of rare-earth ions. Given that Yb has widespread applications among rare-earth elements, we selected Yb 3+ for detection to validate the sensor's performance. The developed electrochemical biosensor exhibits a detection limit of 1.617 μM and demonstrates linear response across a concentration range of 10–90 μM (R 2 = 0.98). This rare-earth ion electrochemical sensor offers multiple advantages, including high sensitivity, a broad detection range, low cost, ease of use, portability, and potential for field deployment. The materials employed are environmentally friendly, aligning with green production requirements. The proposed method holds promise for practical applications in rare earth mineral exploration.
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产品关联
DOI
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2022
·Vol. 45
·期 13
·2334-2343
·
IF 3.614
Hongyuan Liu,Jing Jin,Huifu Xue,Cuicui Guo,Feng Ren,Xiaolin He,Jiping Chen,Chun Hu
Based on the size- and shape-selective sorption, 13X molecular sieves were developed as solid-phase extraction adsorbents to cleanup serum extract for the determination of polybrominated diphenyl ethers. The important parameters affecting the cleanup efficiency were investigated including the amount of sorbents, the type, and volume of solvents. Under the optimized conditions, the capacity for removing impurities was evaluated via gel permeation chromatography and gas chromatography with mass spectrometry. The results demonstrated that up to 99% of lipids in corn oil (13 mg) can be removed after cleanup, and endogenous compounds in serum can also be effectively eliminated. The cleanup efficiency is not only superior to hydrophile-lipophile balance column, but also close to acid silica gel and multifunction impurity sorbents. Generally, the developed cleanup method exhibited higher recovery for polybrominated diphenyl ethers with more than four bromines, especially for nona- and deca-brominated diphenyl ethers (99.1˗117.8%). The cleanup method can be coupled with gas chromatography and tandem mass spectrometry for polybrominated diphenyl ethers analysis in human serum. The method detection limits were 0.01˗0.27 ng/mL and average recovery was 50.9˗113.3%, except 2,3',4',6-tetrabrominated, 2,3',4,4',6-pentabrominated, and 2,3,3',4,4',5',6-heptabrominated diphenyl ethers. 2,2',4,5'-Tetrabrominated diphenyl ethers had the highest detection frequency (95%) in human serum, whereas decabrominated diphenyl ethers had the maximum mean concentration (0.50 ng/mL).
研究领域:
环境科学
·
分析化学
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DOI
PubMed
高影响因子
Foods
·
2024
·Vol. 13
·期 5
·635
·
IF 4.7
Aiping Li,Chen Wang,Zhenghao Wu,Yingying Liu,Zhenxia Hao,Chengyin Lu,Hongping Chen
Ningnanmycin is a widely used antibiotic in agricultural production that effectively controls fungal and viral diseases in tea trees and chrysanthemums. The polarity characteristic of ningnanmycin has posed limitations on the development of robust detection methods, thereby hindering effective monitoring and control measures. By combining cation exchange solid phase extraction (SPE) with hydrophilic interaction chromatography tandem mass spectrometry (HILIC-MS/MS), we have effectively tackled the issue pertaining to the separation and retention of ningnanmycin. The average recoveries of ningnanmycin in green tea, black tea, and chrysanthemum were 77.3–82.0%, 80.1–81.5%, and 74.0–80.0%, respectively. The intraday and interday relative standard deviations (RSDs) were below and equal to 7.7%. Good linearity was observed in the concentration range of 1–1000 μg/L (R2 > 0.998). The limits of detection (LODs) ranged from 1.1 μg/kg to 7.1 μg/kg, and the limits of quantification (LOQs) ranged from 3.6 μg/kg to 23.7 μg/kg for ningnanmycin. These results indicate the good accuracy, repeatability, reproducibility, and sensitivity of the method. It is suitable for detecting ningnanmycin in tea and chrysanthemum.
研究领域:
分析化学
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食品科学
·
植物保护
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产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）