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Biomedical Analysis
About Journal
ISSN:1004-4957
CN:44-1318/TH
Administrator: Guangdong Academy of Sciences
Sponsors: Institute of Analysis,Guangdong Academy of Sciences (Guangzhou Center for Analytical and Testing of China) ; China Association for Instrumental Analysis
Editor-in-Chief: Academician Jiang Guibin
Publication Frequency: Monthly
Tel: 020-87684776
Address: No.100, Xianlie Zhong Road, Guangzhou
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2026年第45卷第10期
- 摘要：In this study，a method was established for the simultaneous determination of short-，medium-，and long-chain chlorinated paraffins（SCCPs，MCCPs，and LCCPs） in soil using ultra-high performance liquid chromatography-electrostatic field orbitrap high resolution mass spectrometry（UPLC-Orbitrap HRMS） for highly sensitive detection. The method is based on a pretreatment procedure involving ultrasonic extraction and multi-layer silica gel column cleanup，coupled with optimization of the extraction solvent type，volume，and extraction frequency. Soil samples were subjected to ultrasonic extraction with a dichloromethane/n-hexane mixture，followed by multi-layer silica gel column cleanup，elution with dichloromethane/n-hexane，and constant-volume adjustment prior to UPLC-Orbitrap HRMS analysis. The chromatographic separation was performed on a Hypersil GOLD VANQUISH C18 column，and mass spectrometric detection was conducted via a heated electrospray ionization（H-ESI） source in the negative ion mode under full-scan acquisition. SCCPs and MCCPs exhibited good linearity over the range between 10-5 000 ng·mL-1，and LCCPs exhibited good linearity over the range between 10-1 000 ng·mL-1，with correlation coefficients（r2） greater than 0.98. The method detection limits（MDLs） for SCCPs，MCCPs，and LCCPs were 18.9，19.7，and 2.06 ng·g-1，respectively. The average recoveries of CPs at low，medium，and high spiked concentration levels ranged between 75.6%-116%，80.5%-99.3%，and 93.1%-109%，with relative standard deviations（RSDs） of 2.2%-9.3%，3.6%-6.5%，and 1.8%-4.6%，respectively. The developed method was applied to analyze CPs in 11 soil samples collected from a typical rubber industrial park. The detection frequencies of SCCPs，MCCPs，and LCCPs were all 100%，with concentration ranges between 48.5-2 490 ng·g-1（mean 682 ng·g-1），82.3-4 090 ng·g-1（mean 1 560 ng·g-1），and 10.7-809 ng·g-1（mean 242 ng·g-1），respectively. MCCPs were identified as the predominant congener group，accounting for 62.7% of the total CPs. This method exhibits good reproducibility and high sensitivity，enabling efficient extraction and accurate quantification of CPs in soil，and can serve as a viable analytical option for environmental monitoring and risk assessment.关键词：chlorinated paraffins（CPs）;soil;ultrasonic extraction;ultra-high performance liquid chromatography-high resolution mass spectrometry（UPLC-HRMS）76|56|0更新时间：2026-10-14
- 摘要：To align with the development trend of green analytical chemistry，this study adopted built-in pure-water electrolysis hydrogen generation technology，and utilizing an unattended mode established a novel analytical method for mercury speciation determination using liquid chromatography-atomic fluorescence spectrometry（LC-AFS）. The experimental results revealed good linearity of the mercury species concentrations in the range of 0-100 μg/L，with correlation coefficients（r） exceeding 0.999. The inorganic mercury，methylmercury，and ethylmercury detection limits were 0.005，0.004，and 0.004 mg/kg，respectively. The methylmercury determination sensitivity was significantly improved compared with that of traditional LC-AFS. The recoveries at different concentration levels ranged from 81.0% to 107%，and the relative standard deviations were less than 5%. The mercury speciation determination results for the certified reference materials，namely，tuna（ERM-CE464） and fish muscle（GBW10029），were both within the range of the certified standard values. Certain deep-sea fish have been shown to contain high levels of methylmercury，which emphasizes the food safety concerns associated with methylmercury in carnivorous fish. Compared with the currently mainstream traditional LC-AFS method for mercury speciation determination，the proposed method significantly reduced the usage of hydrochloric acid，potassium borohydride，and potassium persulfate，and decreased the waste-liquid generation. Additionally，this technique employed a unique concentric-structure semi-shielded rectangular tube，which effectively prevented fluorescence quenching while substantially reducing the argon-gas consumption. Overall，the proposed method is highly sensitive and accurate and suitable for the analysis and determination of mercury speciation in fish aquatic samples. Moreover，this method constitutes a low-cost and environmentally-friendly mercury speciation analysis technique.关键词：liquid chromatography-atomic fluorescence spectrometry;built-in controllable online electrolysis for hydrogen generation;mercury speciation;fish aquatic products76|57|0更新时间：2026-10-14
- 摘要：This study established a novel method for the simultaneous determination of 23 perfluoroalkyl substances（PFASs） in surface water，groundwater，seawater，domestic sewage，and industrial wastewater by combining online solid-phase extraction with large-volume injection technology and high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）. Water samples were prepared for analysis by mixing them with methanol and ammonium acetate（final concentrations：10% methanol and 2 mmol/L ammonium acetate），after which they were filtered and directly injected. Following online enrichment on a WAX column，the analytes were transferred to a C18 analytical column and separated within 14 min by gradient elution using acetonitrile-2 mmol/L ammonium acetate as the mobile phase. The PFASs were detected by tandem mass spectrometry in multiple reaction monitoring（MRM） mode and were quantified using the isotope internal standard method. The 23 target PFASs exhibited good linearity in the range of 0.50-100 ng/L，with all correlation coefficients（r） exceeding 0.998，and detection limits ranging from 0.05 to 0.42 ng/L.The spiked recoveries of 23 target PFASs were 78%-118%，with relative standard deviations of 2.5%-15%. The developed method was used to analyze 14 real water samples collected in Liaoning Province，including surface water，groundwater，seawater，and the effluent of a wastewater treatment plant. Eleven PFASs were detected，with PFBA，PFPeA，PFHxA，PFOA，PFBS，and PFOS being the predominant contaminants. Compared with conventional offline solid-phase extraction methods，this method requires small water samples（only 5 mL） and features a high degree of automation in terms of sample pretreatment. This green analytical technique has several advantageous features：low sample consumption，low solvent usage，broad detectable target spectrum，high analytical efficiency，and excellent environmental compatibility. The new method provides a simple，rapid，and accurate analytical tool for routinely monitoring legacy and emerging PFASs in different types of water environments.关键词：online solid-phase extraction;large-volume injection;high performance liquid chromatography-tandem mass spectrometry;per- and polyfluoroalkyl substances;water83|35|0更新时间：2026-10-14
- 摘要：To meet the need for the simultaneous determination of three brominated flame retardants in soil，namely tetrabromobisphenol A-bis（2，3-dibromo-2-methylpropyl ether）（TBBPA-DBMPE），decabromodiphenyl ethane（DBDPE），and hexabromocyclododecane（HBCD），this study compared the extraction efficiencies of accelerated solvent extraction and ultrasonic extraction，optimized the extraction solvent and purification conditions of the composite silica-gel column，and further optimized the chromatographic and mass spectrometric parameters based on the separation performance and mass spectrometric responses of the target analytes，thereby developing an ultra-performance liquid chromatography-tandem triple-quadrupole mass spectrometry（UPLC-MS/MS） method for the determination of TBBPA-DBMPE，DBDPE，and the three major diastereoisomers of HBCD in soil. In the concentration range of 2-500 ng·mL-1 for TBBPA-DBMPE and HBCD and 10-2 500 ng·mL-1 for DBDPE，the linearity exhibited correlation coefficients（r2）>0.999. When the soil sample mass was 20 g and injection volume 5 μL，the detection limits of the method were 0.004-0.02 ng·g-1，and the quantitation limits were 0.02-0.05 ng·g-1. At the spiked levels of 0.1，0.5，and 1.0 ng·g-1 for TBBPA-DBMPE and HBCD，and 1，5，and 10 ng·g-1 for DBDPE，the recoveries of TBBPA-DBMPE，DBDPE，and HBCD were 103%-114%，103%-118%，and 73.3%-118%，respectively，with relative standard deviations of 7.1%-7.9%，5.7%-9.7%，and 5.8%-16%，respectively. The proposed method was used to analyze four surface-soil samples collected around a brominated flame-retardant production enterprise in Shandong Province. The concentrations were <0.05-16 ng·g-1 for TBBPA-DBMPE，52-85 ng·g-1 for DBDPE，and 24.4-120.4 ng·g-1 for HBCD. This method is sensitive and reproducible，and suitable for the quantitative trace analysis of brominated flame retardants in environmental soil samples.关键词：brominated flame retardants;soil;TBBPA-DBMPE;DBDPE;HBCD;UPLC-MS/MS53|21|0更新时间：2026-10-14
- 摘要：An analytical method was established for the simultaneous determination of 16 polycyclic aromatic hydrocarbons（PAHs） and 31 n-alkanes in soil with a high petroleum hydrocarbon background by column‑free matrix solid‑phase dispersion-assisted pressurized fluid extraction coupled with gas chromatography-tandem mass spectrometry（CFMSPD-PFE/GC-MS/MS）.Using single‑factor experiments，the optimal ratio of matrix solid‑phase dispersant（silica gel adsorbent） to sample was determined to be 0.5∶1-2∶1. Using an L₁₆（4⁴） orthogonal experiment，the optimized pressurized fluid extraction parameters were set as follows：extraction solvent：n‑hexane/acetone mixture（2∶1，volume ratio），extraction temperature：100 ℃，static extraction time：5 min，and number of extraction cycles：2. The results indicate that PAHs and n-alkanes have favorable linearity within the concentration ranges of 1.0-250 μg/L and 10-2 500 μg/L，respectively，with correlation coefficients r≥0.995 4. The limits of detection were 0.08-0.31 μg/kg and 1.07-3.19 μg/kg，while the corresponding limits of quantification were 0.32-1.24 μg/kg and 4.28-12.8 μg/kg. The average recoveries at three spiked concentration levels ranged from 77.1% to 111%，with relative standard deviations of 2.4-13%. The developed method was applied to the determination of 30 soil samples with petroleum hydrocarbon contents of 865-2 286 mg/kg. The mass concentrations of PAHs and n-alkanes were in the ranges of 2.93-1.50×105 μg/kg and 20.8-5.76×103 μg/kg，respectively. With the advantages of simple operation，short pretreatment procedure，and high sensitivity，the method proposed herein is suitable for the simultaneous analysis of 16 PAHs and 31 n-alkanes in soil with high petroleum hydrocarbon background.关键词：column-free matrix solid-phase dispersion;pressurized fluid extraction;gas chromatography-tandem mass spectrometry;soil;polycyclic aromatic hydrocarbons;n-alkanes73|36|0更新时间：2026-10-14
- 摘要：Online solid-phase extraction-liquid chromatography-triple quadrupole mass spectrometry was established to simultaneously determine 28 pesticide residues in drinking water. Three solid-phase extraction cartridges，namely，hydrophilic-lipophilic balance（HLB），C18，and weak anion exchange（WAX），were compared based on adsorption mechanisms，and HLB was identified as the best extraction cartridge. Extraction parameters were optimized via single-factor experiments，and the optimal conditions were determined as follows：water sample pH：5.0，sample loading volume：10 mL，sample loading flow rate：2 mL/min，and elution with 90% acetonitrile-2 mmol/L ammonium acetate-0.1% formic acid solution at a flow rate of 0.2 mL/min. The methodological validation results showed that the 28 target compounds exhibited good linearity within the range of 0.025-10 μg/L（r≥0.997 9），with the limits of detection and quantification being 0.003-0.010 μg/L and 0.012-0.040 μg/L，respectively. Recoveries at three spiked levels ranged from 80.3% to 114%，with relative standard deviations of 1.4%-14%. The method was applied to analyze 20 drinking water samples. Acephate，bentazone，2，4-D，acetochlor，and chlorantraniliprole were detected at relatively high concentrations，whereas the other target analytes were observed at low concentrations. This sensitive and accurate method is suitable for the simultaneous analysis of 28 pesticide residues in drinking water.关键词：online solid-phase extraction;liquid chromatography-triple quadrupole mass spectrometry;drinking water;pesticide residues;multiresidue determination91|41|0更新时间：2026-10-14
- 摘要：To achieve rapid screening and accurate identification of illegal additions and controlled drugs in multi-scenario applications，a rapid detection method based on atmospheric solids analysis-probe single-quadrupole mass spectrometry（ASAP-MS） was developed in this study. Focusing on antibiotics，glucocorticoids，anesthetics，antifungal agents，psychotropic substances，and novel psychoactive substances，this study optimized the cone voltage parameters to acquire characteristic mass spectral information for each target compound under various voltage conditions，establishing an ASAP-MS rapid-detection database covering 111 target compounds. Library matching between the sample mass spectra and the in-house database was performed using LiveID software，and the screening results were further verified using high-resolution mass spectrometry. Application of this method successfully identified target compounds such as lidocaine and diazepam in real samples，including disinfectant products and samples seized by law enforcement. This method requires facile sample pretreatment，offers high analytical efficiency，and allows flexible database expansion. This enables the rapid screening of large sample volumes and meets the detection requirements of public safety fields，such as market regulation，customs inspection，and drug control enforcement，demonstrating its good application value and broad potential for promotion.关键词：ASAP-MS;illegal additions;controlled drugs;rapid detection;public safety50|26|0更新时间：2026-10-14
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- 0 2 Recent Advances in the Application of Machine Learning in Environmental Analysis and Detection 3694
- 0 3 Recent Progress in Nuclear Radiation Detection Technology and Device 3333
- 0 4 Advances in Tissue Penetration by Optical Imaging Techniques 3161
- 0 5 Research Progress and Prospects of Sonodynamic Therapy 2951
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