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

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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

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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Shukri, D. S. M., Sanagi, M. M., Ibrahim, W. A. W., Abidin, N. N. Z., & Aboul-Enein, H. Y. (2015) · Chromatographia · doi:10.1007/s10337-015-2920-0 · Cited by 33
“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
Novel extraction method based on the dispersion of the extraction solvent for extraction of letrozole from biological fluids
Rezaee, M. B., Yamini, Y., Hojjati, M., & Faraji, M. (2010) · Analytical Methods · doi:10.1039/c0ay00131g · Cited by 33
Magnetic solid-phase extraction followed by high performance liquid chromatography for determination of hexanal and heptanal in human urine
Song, D., Gu, Y., Lü, L., Ai, Z., Zhang, L., & Xu, H. (2011) · Analytical Methods · doi:10.1039/c1ay05102d · Cited by 30
Self-citation
Development of a Efficient and Sensitive Dispersive Liquid–Liquid Microextraction Technique for Extraction and Preconcentration of 10 β2-Agonists in Animal Urine
Li, Y., Zhang, W., Wang, R.-G., Wang, P., & Su, X.-O. (2015) · PLoS ONE · doi:10.1371/journal.pone.0137194 · Cited by 27
“In addition, DLLME has also been used for the extraction of drugs [44, 45] and biomarkers [46] from biological samples such as blood and urine.”
Method
Micro-scale quantitation of ten phthalate esters in water samples and cosmetics using capillary liquid chromatography coupled to UV detection: effective strategies to reduce the production of organic waste
Feng, C.-H., & Jiang, S.-R. (2012) · Microchimica Acta · doi:10.1007/s00604-012-0761-1 · Cited by 27
Simultaneous determination of seven endogenous aldehydes in human blood by headspace gas chromatography-mass spectrometry.
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Determination of the rare earth elements La, Eu, and Yb using solidified floating organic drop microextraction and electrothermal vaporization ICP-MS
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“simplicity, rapidity, low cost, consumption of small organic solvent and high enrichment factor, SFODME has been successfully employed for the determination of organic analytes [16–19], and recently extended to the determination of trace elements [20–26].”
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
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
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
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
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
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 39
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
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
“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
“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
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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
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Aravapally, P. S. N., Chandrasekar, N., Verma, A., & Shah, R. P. (2025) · Bioanalysis · doi:10.1080/17576180.2025.2486929 · Cited by 16
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Dadfarnia, S., Shabani, A. M. H., Esfahani, G. S., & Kazemi, E. (2016) · Spectroscopy Letters · doi:10.1080/00387010.2015.1104359 · Cited by 12
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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
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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
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
Volatile Organic Compounds and the Potential for a Lung Cancer Breath Test
Barash, O., Tisch, U., & Haick, H. (2013) · Lung Cancer Management · doi:10.2217/lmt.13.58 · Cited by 13
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
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
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
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.
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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
“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
“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
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
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
“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

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 › Analytical Chemistry › 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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