Analysis of volatile aldehyde biomarkers in human blood by derivatization and dispersive liquid–liquid microextraction based on solidification of floating organic droplet method by high performance liquid chromatography

Lili, Lv; Xu, Hui; Song, Dandan; Cui, Yanfang; Hu, Sheng; Zhang, Ganbing

doi:10.1016/j.chroma.2010.01.081

Cited by 123Analytical chemistry methods developmentAnalytical Chemistry and ChromatographyMicrofluidic and Capillary Electrophoresis Applications

Analysis of volatile aldehyde biomarkers in human blood by derivatization and dispersive liquid–liquid microextraction based on solidification of floating organic droplet method by high performance liquid chromatography

Lili, Lv, Xu, Hui, Song, Dandan, Cui, Yanfang, Hu, Sheng, Zhang, Ganbing·2010·Journal of Chromatography A

DOI 10.1016/j.chroma.2010.01.081

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Abstract

A new dispersive liquid-liquid microextraction based on solidification of floating organic droplet method (DLLME-SFO) was developed for the determination of volatile aldehyde biomarkers (hexanal and heptanal) in human blood samples. In the derivatization and extraction procedure, 2,4-dinitrophenylhydrazine (DNPH) as derivatization reagent and formic acid as catalyzer were injected into the sample solution for derivatization with aldehydes, then the formed hydrazones was rapidly extracted by dispersive liquid-liquid microextraction with 1-dodecanol as extraction solvent. After centrifugation, the floated droplet was solidified in an ice bath and was easily removed for analysis. The effects of various experimental parameters on derivatization and extraction conditions were studied, such as the kind and volume of extraction solvent and dispersive solvent, the amount of derivatization reagent, derivatization temperature and time, extraction time and salt effect. The limit of detections (LODs) for hexanal and heptanal were 7.90 and 2.34nmolL(-1), respectively. Good reproducibility and recovery of the method were also obtained. The proposed method is an alternative approach to the quantification of volatile aldehyde biomarkers in complex biological samples, being more rapid and simpler and providing higher sensitivity compared with the traditional dispersive liquid-liquid microextraction (DLLME) methods.

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Lv et al. [30] used LPME-SFO method combined with derivatization for the determination of hexanal and heptanal in human blood samples via HPLC.
“Lv et al [30] used LPME-SFO method combined with derivatization for the determination of hexanal and heptanal in human blood samples via HPLC.”
From Developments in Liquid-phase Microextraction Method Based on Solidification of Floating Organic Drop (2010) · cites this paper as [30]
For the LPME-SFO-HPLC determination of hexanal and heptanal in human blood samples, the recoveries of the target analytes from real samples were 67.8%-70.2%.
“The recoveries of the target analytes from real samples were 67.8%-70.2%.”
From Developments in Liquid-phase Microextraction Method Based on Solidification of Floating Organic Drop (2010) · cites this paper as [30]
For the LPME-SFO-HPLC determination of hexanal and heptanal in human blood samples, the RSDs of intraday and inter-day were below 4.11% and 2.91%, respectively.
“The RSDs of intraday and inter-day were below 4.11% and 2.91%, respectively.”
From Developments in Liquid-phase Microextraction Method Based on Solidification of Floating Organic Drop (2010) · cites this paper as [30]

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Background
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Method
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Background
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“This convenient and inexpensive technique has been widely used for extraction of metals [20–22], polycyclic aromatic hydrocarbons [23], volatile aldehyde biomarkers [24], steroid hormones [25], pesticides [26], and polychlorinated biphenyls [27].”
Method
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Self-citation
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Method
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Method
Chromatographic determination of aliphatic aldehydes in human serum after pre-column derivatization using 2,2′-furil, a novel fluorogenic reagent
Ali, M. F. B., Kishikawa, N., Ohyama, K., Mohamed, H. A.-M., Abdel-Wadood, H. M., Mohamed, A. M., & Kuroda, N. (2013) · Journal of Chromatography A · doi:10.1016/j.chroma.2013.03.033 · Cited by 29 · see citing works
Derivatization and Solidification of Floating Dispersive Liquid‐phase Microextraction for the Analysis of Kanamycin in Wastewater and Soil by HPLC with Fluorescence Detection
Hu, S., Song, Y., Bai, X., Jiang, X., & Yang, X. (2013) · CLEAN - Soil Air Water · doi:10.1002/clen.201200374 · Cited by 24 · see citing works
Self-citation
Development of solvent micro-extraction combined with derivatization
Lin, H., Wang, J., Zeng, L., Li, G., Sha, Y., Da, W., & Liu, B. (2013) · Journal of Chromatography A · doi:10.1016/j.chroma.2013.04.039 · Cited by 29 · see citing works
Microspectrophotometric determination of erythrosine in beverage and water samples after ultrasonic assisted supramolecular-based dispersion solidification liquid–liquid microextraction
Shokrollahi, A., Pili, H. B., & Hemmatidoust, K. (2017) · Journal of Analytical Chemistry · doi:10.1134/s1061934817060028 · Cited by 27 · see citing works
Determination of organic pollutants in coking wastewater by dispersive liquid–liquid microextraction/ GC / MS
Song, G., Zhu, C., Hu, Y., Chen, J., & Cheng, H. (2013) · Journal of Separation Science · doi:10.1002/jssc.201201151 · Cited by 24 · see citing works
Dispersive Liquid–Liquid Microextraction
Assadi, Y., Farajzadeh, M. A., & Bidari, A. (2012) · Elsevier eBooks · doi:10.1016/b978-0-12-381373-2.00051-x · Cited by 36 · see citing works
2,4-dinitrophenylhydrazine capturing combined with mass defect filtering strategy to identify aliphatic aldehydes in biological samples
Wang, S., Liu, H., Zhu, J., Zhou, S.-S., Xu, J., Zhou, J., Mao, Q., Kong, M., Li, S., & Zhu, H. (2022) · Journal of Chromatography A · doi:10.1016/j.chroma.2022.463405 · Cited by 18 · see citing works
Determination of Sudan Dyes in Juice Samples via Solidification of Ionic Liquid in Microwave-Assisted Liquid-Liquid Microextraction Followed by High-Performance Liquid Chromatography
Hu, M.-Z., Wu, L.-J., Song, Y., Li, Z.-C., Ma, Q., Zhang, H.-Q., & Wang, Z.-M. (2016) · Food Analytical Methods · doi:10.1007/s12161-015-0389-y · Cited by 19 · see citing works
“The addition of salt to the extract is usually made to improve the enrichment efficiency of the analytes because the increased ionic strength of aqueous phase could aid the partition of analytes to organic phase (Lv et al. 2010).”
Background
Liquid-phase microextraction of biomarkers: A review on current methods
Hamidi, S., & Alipour-Ghorbani, N. (2017) · Journal of Liquid Chromatography & Related Technologies · doi:10.1080/10826076.2017.1374291 · Cited by 24 · see citing works
“This method was developed for the determination of volatile aldehyde biomarkers (hexanal and heptanal) in human blood samples.([38]) Salivary mercury can be used as a biomarker for mercury exposure and cold vapor atomic SFODME coupled to fluorescence spectrometry was used for its quantification in ultratrace levels.”
Method
Application of solidified floating organic drop microextraction method for biomonitoring of chlorpyrifos and its oxon metabolite in urine samples.
Pelit, F., & Yengin, Ç. (2014) · Journal of chromatography. B, Analytical technologies in the biomedical and life sciences · doi:10.1016/j.jchromb.2014.01.004 · Cited by 18
Screening of a highly effective fluorescent derivatization reagent for carbonyl compounds and its application in HPLC with fluorescence detection
Chen, L., Fu, Y., Fang, W.-L., Guo, X., & Wang, H. (2018) · Talanta · doi:10.1016/j.talanta.2018.04.017 · Cited by 22 · see citing works
A dispersive liquid-liquid microextraction method based on the solidification of a floating organic drop combined with HPLC for the determination of lovastatin and simvastatin in rat urine.
Zhao, L.-S., Zhao, P., Wang, L.-L., Ma, X.-W., Hou, X., & Li, F. (2014) · Biomedical chromotography · doi:10.1002/bmc.3205 · Cited by 16 · see citing works
Modified dispersive liquid-liquid microextraction for pre-concentration of benzene, toluene, ethylbenzene and xylenes prior to their determination by GC
Faraji, H., Feizbakhsh, A., & Helalizadeh, M. (2013) · Microchimica Acta · doi:10.1007/s00604-013-1037-0 · Cited by 15 · see citing works
Strategic approaches to assess and quantify the oxidative stress biomarkers in complex biological systems
Aravapally, P. S. N., Chandrasekar, N., Verma, A., & Shah, R. P. (2025) · Bioanalysis · doi:10.1080/17576180.2025.2486929 · Cited by 16 · see citing works
Micro-solid phase extraction followed by thermal extraction coupled with gas chromatography-mass selective detector for the determination of polybrominated diphenyl ethers in water.
Naing, N., Li, S. F., & Lee, H. K. (2016) · Journal of Chromatography A · doi:10.1016/j.chroma.2016.06.056 · Cited by 13
Dispersive liquid–liquid microextraction based on solidification of floating organic drop for separation and preconcentration of malachite green before its determination by flow injection spectrophotometry
Dadfarnia, S., Shabani, A. M. H., Esfahani, G. S., & Kazemi, E. (2016) · Spectroscopy Letters · doi:10.1080/00387010.2015.1104359 · Cited by 12 · see citing works
Review—Recent Advances in Direct and Indirect Methods for Sensing Carbonyl Compounds Aldehydes in Environment and Foodstuffs
Laghrib, F., Lahrich, S., & Mhammedi, M. A. E. (2019) · Journal of the Electrochemical Society · doi:10.1149/2.0761915jes · Cited by 12
Cyclohexane‐1,3‐dione as a derivatizing agent for the analysis of aldehydes by micelar electrokinetic chromatography with diode array detection
Donegatti, T. A., Lobato, A., Gonçalves, L. M., & Pereira, E. A. (2019) · Electrophoresis · doi:10.1002/elps.201900171 · Cited by 11
A novel sorptive extraction method based on polydimethylsiloxane frit for determination of lung cancer biomarkers in human serum.
Xu, H., & Wang, S.-Y. (2012) · Analytica Chimica Acta · doi:10.1016/j.aca.2012.02.046 · Cited by 11
Self-citation
Recent Advances in Liquid Microextraction Techniques Coupled With Ms For Determination of Small-Molecule Drugs in Biological Samples
Saraji, M., & Khaje, N. (2012) · Bioanalysis · doi:10.4155/bio.12.26 · Cited by 11 · see citing works
Microwave-assisted liquid–liquid microextraction based on solidification of floating organic droplet for the determination of triazines in honey samples
Hu, M.-Z., Wu, L.-J., Song, Y., Li, Z.-C., Ma, Q., Zhang, H.-Q., & Wang, Z.-M. (2015) · Analytical Methods · doi:10.1039/c5ay01963j · Cited by 10 · see citing works
Volatile organic compounds and the potential for a lung cancer breath test
Barash, O., Tisch, U., & Haick, H. (2013) · doi:10.2217/lmt.13.58 · Cited by 10
Dispersive liquid–liquid microextraction for the high performance liquid chromatographic determination of aldehydes in cigarette smoke and injectable formulations
Tabrizi, A. B., & Abdollahi, A. A. (2013) · Journal of Hazardous Materials · doi:10.1016/j.jhazmat.2013.03.034 · Cited by 10 · see citing works
Dispersive Liquid–Liquid Extraction Based on Freezing of the Organic Drop, Followed by GC for the Determination of Methyl Methacrylate in Wastewater
Mokhtari, B., Dalali, N., & Pourabdollah, K. (2013) · Chromatographia · doi:10.1007/s10337-013-2403-0 · Cited by 10 · see citing works
Improved solid-phase extraction/micellar procedure for the derivatization/preconcentration of benzaldehyde and methyl derivatives from water samples.
Fernández-Molina, J. M., & Silva, M. (2011) · Talanta: The International Journal of Pure and Applied Analytical Chemistry · doi:10.1016/j.talanta.2011.04.004 · Cited by 10
Supramolecular based-ligandless ultrasonic assisted-dispersion solidification liquid–liquid microextraction of uranyl ion prior to spectrophotometric determination with dibenzoylmethane
Shokrollahi, A., & Pili, H. B. (2016) · RSC Advances · doi:10.1039/c5ra23355k · Cited by 10 · see citing works
Dynamic microwave-assisted extraction combined with liquid phase microextraction based on the solidification of a floating drop for the analysis of organochlorine pesticides in grains followed by GC
Li, G.-J., Zhang, X., Liu, T.-T., Fan, H.-X., Liu, H.-C., Li, S., Wang, D.-W., & Ding, L. (2021) · doi:10.1016/j.fshw.2021.02.029 · Cited by 9
Electrospun polystyrene nanofibers as a novel adsorbent to transfer an organic phase from an aqueous phase.
Liu, F., Song, D.-D., Huang, X., & Xu, H. (2016) · Journal of Separation Science · doi:10.1002/jssc.201501182 · Cited by 9 · see citing works
Self-citation
Determination of Flavonoids by Solidification of Floating Organic Drop Liquid-Phase Microextraction and High-Performance Liquid Chromatography
Xue, X., Zhao, Z., Li, Q., Wang, D., Xu, X., Zhu, L., & Yang, D. (2016) · Analytical Letters · doi:10.1080/00032719.2016.1149859 · Cited by 10 · see citing works
“However, dispersive liquid–liquid microextraction based on solidification of floating organic drop has been widely studied (Asadollahi, Dadfarnia, and Shabani 2010; Li et al. 2010; Yamini et al. 2010; Moghadam, Shabani, and Dadfarnia 2011; Chung, Leong, and Huang 2012; Wang et al. 2014; Hashemi et al. 2015) due to its…”
Background
Multiple objective optimization of air assisted liquid-liquid microextraction combined with solidified floating organic drop microextraction for simultaneous determination of trace copper and nickel
ISLAMI-BONAB, F., Sajedi‐Amin, S., Sorouraddin, S. M., Maleknia, S. D., & Naseri, A. (2021) · TURKISH JOURNAL OF CHEMISTRY · doi:10.3906/kim-2010-24 · Cited by 8 · see citing works
“These shortcomings were resolved with the use of a disperser solvent, resulting in the development of DLLME-SFOD [10,21,22], and further by introducing ultrasound emulsification microextraction and air agitation as efficient and preferable dispersion techniques, USAEME-SFOD [23–25] and AALLME-SFOD…”
Optimization of alcohol-assisted dispersive liquid-liquid microextraction by experimental design for the rapid determination of fluoxetine in biological samples.
Hamedi, R., & Hadjmohammadi, M. (2016) · Journal of Separation Science · doi:10.1002/jssc.201600667 · Cited by 8 · see citing works
Application of dispersive liquid–liquid microextraction with alcoholic solvents followed by HPLC–UV as a sensitive and efficient method for the extraction and determination of citalopram in biological samples using an experimental design
Hamedi, R., & Hadjmohammadi, M. (2017) · Journal of the Iranian Chemical Society · doi:10.1007/s13738-017-1048-6 · Cited by 7 · see citing works
Microextraction of Furosemide from Human Serum and Its Fluorimetric Determination
Rezazadeh, A., Amjadi, M., Manzoori, J. L., Ghaffari, A., & Jouyban, A. (2018) · Pharmaceutical Sciences · doi:10.15171/ps.2018.11 · Cited by 4 · see citing works
“Selection of extraction solvent Several factors such as higher density in comparison with water, low solubility in water and high extraction capability of interested compounds should be considered for selection of extraction solvent.(44) Chloroform, dichloromethane, carbon tetrachloride and 1,2dichlorobenzol were stud…”
Background
Response surface methodology for the optimization of dispersive liquid–liquid microextraction of chloropropanols in human plasma
Gonzalez‐Siso, P., Lorenzo, R. A., Regenjo, M., Fernández, P., & Carro, A. M. (2015) · Journal of Separation Science · doi:10.1002/jssc.201500468 · Cited by 7 · see citing works

Authors: Lili, L., Xu, H., Song, D., Cui, Y., Hu, S., & Zhang, G.
Affiliations: Central China Normal University (CN)
Hubei Cancer Hospital (CN)
Hubei University (CN)
Corresponding author: Xu, Hui
Zhang, Ganbing
ORCID: Xu, Hui
Song, Dandan
Cui, Yanfang
Hu, Sheng
Zhang, Ganbing
Venue: Journal of Chromatography A
Publisher: Elsevier BV
Published: 2010-04
Volume: 1217
Issue: 16
Pages: 2365-2370
ISSN: 0021-9673 (ISSN-L)
DOI: 10.1016/j.chroma.2010.01.081
OpenAlex: W2093027155
Cited by: 123
References: 0
Citations by year: 2026: 5 · 2025: 2 · 2024: 1 · 2023: 3 · 2022: 4 · 2021: 3 · 2020: 1 · 2019: 8 · 2018: 4 · 2017: 5 · 2016: 10 · 2015: 12 · 2014: 6 · 2013: 20 · 2012: 17
FWCI: 18.74
Type: journal article
Language: en
Open access: closed
Licence: www.elsevier.com/tdm/userlicense/1.0/ (tdm)
Locations: Journal of Chromatography A (publishedVersion)
PubMed (publishedVersion)
Topics: Physical Sciences › Chemistry › Analytical Chemistry › Analytical chemistry methods development
Physical Sciences › Chemistry › Spectroscopy › Analytical Chemistry and Chromatography
Physical Sciences › Engineering › Biomedical Engineering › Microfluidic and Capillary Electrophoresis Applications
Keywords: hexanal, heptanal, human blood, dispersive liquid-liquid microextraction, solidification of floating organic droplet, 2,4-dinitrophenylhydrazine derivatization, hydrazones, derivatization optimization, oxidative stress biomarkers
MeSH terms: Aldehydes, Chromatography, High Pressure Liquid, Chemical Fractionation, Humans, Dodecanol, Phenylhydrazines, Sensitivity and Specificity, Sodium Chloride, Solvents, Time, Reproducibility of Results, Linear Models, Volatile Organic Compounds

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Analysis of volatile aldehyde biomarkers in human blood by derivatization and dispersive liquid–liquid microextraction based on solidification of floating organic droplet method by high performance liquid chromatography

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