Application and optimization of microwave-assisted extraction and dispersive liquid–liquid microextraction followed by high-performance liquid chromatography for sensitive determination of polyamines in turkey breast meat samples

doi:10.1016/j.foodchem.2015.06.079

Food Chemistry

Volume 190, 1 January 2016, Pages 1168-1173

https://doi.org/10.1016/j.foodchem.2015.06.079 Get rights and content

Highlights

•
A new method was developed to determine of three polyamines from food sample.
•
MAE–DLLME was used for pre-concentration of three poly amines from matrix sample.
•
Final separation and quantification was performed by HPLC–UV.
•
The increased sensitivity in use the MAE–DLLME–HPLC–UV has been demonstrated.

Abstract

A novel method based on microwave-assisted extraction and dispersive liquid–liquid microextraction (MAE–DLLME) followed by high-performance liquid chromatography (HPLC) was developed for the determination of three polyamines from turkey breast meat samples. Response surface methodology (RSM) based on central composite design (CCD) was used to optimize the effective factors in DLLME process. The optimum microextraction efficiency was obtained under optimized conditions. The calibration graphs of the proposed method were linear in the range of 20–200 ng g⁻¹, with the coefficient determination (R²) higher than 0.9914. The relative standard deviations were 6.72–7.30% (n = 7). The limits of detection were in the range of 0.8–1.4 ng g⁻¹. The recoveries of these compounds in spiked turkey breast meat samples were from 95% to 105%. The increased sensitivity in using the MAE–DLLME–HPLC–UV has been demonstrated. Compared with previous methods, the proposed method is an accurate, rapid and reliable sample-pretreatment method.

Introduction

Dietary polyamines (PA) (putrescine, spermidine, and spermine) are low molecular weight bases with an aliphatic structure, which used to be classified within the group of biogenic amines (BA) (Ladero, Calles-Enríquez, Fernández, & Alvarez, 2010). However, they were considered separately as an individual compounds in 1990s, due to their roles in the growth and function of normal cells as well as their mode of formation (Kalač, 2009). Polyamines are ubiquitous among all different living organisms from bacteria to mammals (Kalač, 2014). They can also be found in different foodstuffs including wine, fruit, vegetables, cheese, different types of meat such as beef and fish in low concentrations (Naila, Flint, Fletcher, Bremer, & Meerdink, 2010). These components have controversial influences on human health as they can be useful for growth and wounds’ healing, while can be harmful as they accelerate the growth of tumors (Dadáková, Pelikánová, & Kalač, 2012). Because there is a controversy over exposure levels of polyamines in human body, it is very important to develop an efficient method for determination of these compounds in different foodstuffs.

Different methods have been used for analyzing BAs and PAs in foods, such as gas chromatography (GC) (Almeida, Fernandes, & Cunha, 2012), thin-layer chromatography (TLC) (Jeya Shakila, Vasundhara, & Kumudavally, 2001), capillary electrophoretic method (CE) (Lange, Thomas, & Wittmann, 2002), ion chromatography–mass spectrometry (IC–MS) (Saccani, Tanzi, Pastore, Cavalli, & Rey, 2005), ultra-performance liquid chromatography (UPLC) (Dadáková, Křížek, & Pelikánová, 2009) and high performance liquid chromatography (HPLC) (Önal, 2007). HPLC requires minimal preparation and it has high selectivity and sensitivity (Huang et al., 2009); therefore this method has been widely used for determination of BAs in different kinds of food (Lavizzari, Teresa Veciana-Nogués, Bover-Cid, Mariné-Font, & Carmen Vidal-Carou, 2006). However, direct determination of PAs (lipophilic compounds), especially in fat and protein-rich food such as meat or meat products is impossible and multi-step sample-preparation procedures are necessary to isolate PAs. (Triki, Jimenez-Colmenero, Herrero, & Ruiz-Capillas, 2012). Owing to this fact, recent trend is to develop efficient, economical, and miniaturized sample preparation techniques (Chaichi et al., 2013, Ghasemzadeh-Mohammadi et al., 2012). Conventional liquid–liquid extraction (LLE) and solid-phase extraction (SPE) are widely used for pre-concentration and clean-up before analysis. These methods have disadvantages such as time consuming and tedious and often need significant amounts of potentially toxic solvents (Almeida et al., 2012).

Recently, a novel sample preparation technique dispersive liquid–liquid microextraction (DLLME) was developed by Assadi and co-workers in 2006 (Rezaee et al., 2006). It is based on a ternary component solvent system like homogeneous liquid–liquid extraction (HLLE) and cloud point extraction (CPE). The advantages of the DLLME technique are fast, high recovery and selectivity, simplicity of operation, good sensitivity and low cost (Kamankesh et al., 2015, Pena-Pereira et al., 2012). The DLLME technique is a powerful method in separation of different analytes in complex matrices. Additionally, it is able to eliminate matrix interference (Ghasemzadeh-Mohammadi et al., 2012, Madani-Tonekaboni et al., 2015, Nojavan et al., 2015). The technique can be applied in most laboratories as well as it is compatible with different analytical methods such as gas chromatography (GC), high-performance liquid chromatography (HPLC), electrothermal atomic absorption spectrometry (Kamankesh et al., 2013, Mohammadi et al., 2013, Ramezani et al., 2014).

In this study, a new analytical method for separation and determination of three polyamines including putrecine, spermidine and spermine using dispersive liquid–liquid microextraction (DLLME) followed by HPLC with UV detector was investigated. A binary system comprises the extracting solvents (1-octanol and acetonitrile) and the sample solution was applied for the sample extraction. The extraction conditions were optimized using RSM based on CCD. The developed method was successfully applied for the accurate determination of traces amount of polyamines in turkey breast meat samples and satisfactory results were obtained.

Section snippets

Reagents, materials and standards

The turkey breast meat samples (white turkey hybrid breeds) were purchased from a local supermarket (Tehran, Iran), and stored at 4°C. Polyamine standards including putrescine dihydrochloride, spermidine trihydrochlride, spermine tetrahydrochloride and derivative reagent dansyl chloride were obtained from Sigma–Aldrich (St. Louis, MO, USA). Acetonitrile, acetone, methanol and HPLC-grade water were purchased from Dae Jung (South Korea). Hydrochloric acid (HCl) (37%, w/w), sodium hydroxide

Results and discussion

Optimal separation and detection of three polyamines, namely putrecine, spermidine and spermine in turkey breast meat samples was obtained by optimizing four important variables (volume of extraction solvent, volume of disperser solvent, amount of salt and sample pH) influencing the DLLME process. Response surface methodology was used for optimization of the extraction efficiency of DLLME method. The selection of a suitable organic solvent is very important for DLLME process. A high

Conclusion

In this study, a new, efficient and reliable method was developed to extract and analyze polyamines in turkey breast meat using MAE–DLLME–HPLC. RSM based on CCD offers the best experimental conditions with the minimum number of experiments was applied to optimize and determine the interaction and quadratic effects of important parameters on the performance of microextraction process. In comparison to other methods, the proposed method has significant advantages including low consumption of

Acknowledgment

The authors would like to thank the National Nutrition and Food Technology Research Institute of Iran for financial support of this work.

References (25)

C. Almeida et al.
A novel dispersive liquid–liquid microextraction (DLLME) gas chromatography–mass spectrometry (GC–MS) method for the determination of eighteen biogenic amines in beer
Food Control
(2012)
M. Chaichi et al.
Optimization and application of headspace liquid-phase microextraction coupled with gas chromatography–mass spectrometry for determination of furanic compounds in coffee using response surface methodology
Microchemical Journal
(2013)
E. Dadáková et al.
Determination of biogenic amines in foods using ultra-performance liquid chromatography (UPLC)
Food Chemistry
(2009)
E. Dadáková et al.
Contents of biologically active polyamines in duck meat and giblets after slaughter and their changes during meat storage and cooking
Food Research International
(2012)
G. Favaro et al.
Determination of biogenic amines in fresh and processed meat by ion chromatography and integrated pulsed amperometric detection on Au electrode
Food Chemistry
(2007)
V. Ghasemzadeh-Mohammadi et al.
Microwave-assisted extraction and dispersive liquid–liquid microextraction followed by gas chromatography–mass spectrometry for isolation and determination of polycyclic aromatic hydrocarbons in smoked fish
Journal of Chromatography A
(2012)
K.-J. Huang et al.
Ultrasound-assisted dispersive liquid–liquid microextraction combined with high-performance liquid chromatography–fluorescence detection for sensitive determination of biogenic amines in rice wine samples
Journal of Chromatography A
(2009)
R. Jeya Shakila et al.
A comparison of the TLC-densitometry and HPLC method for the determination of biogenic amines in fish and fishery products
Food Chemistry
(2001)
P. Kalač
Health effects and occurrence of dietary polyamines: A review for the period 2005–mid 2013
Food Chemistry
(2014)
M. Kamankesh et al.
Rapid determination of polycyclic aromatic hydrocarbons in grilled meat using microwave-assisted extraction and dispersive liquid–liquid microextraction coupled to gas chromatography–mass spectrometry
Meat Science
(2015)

M. Kamankesh et al.

Dispersive liquid–liquid microextraction followed by high-performance liquid chromatography for determination of benzoate and sorbate in yogurt drinks and method optimization by central composite design

Talanta

(2013)

J. Lange et al.

Comparison of a capillary electrophoresis method with high-performance liquid chromatography for the determination of biogenic amines in various food samples

Journal of Chromatography B

(2002)

Cited by (40)

Current sample preparation strategies for the chromatographic and mass spectrometric determination of furfural compounds
2023, Microchemical Journal
Furfural compounds, formed during food storage and processing, are widely existed in food samples. Formation of furfural compounds may affect the safety and quality of foods. Thus, many countries and organizations have issued policies to limit the maximum content of furfural compounds. Therefore, it is necessary to develop analytical methods to monitor the concentration of furfural compounds in foods. However, the direct instrumental analysis of furfural compounds in foods is a continuous challenge, mainly because of complex samples and large amounts of co-existing interfering substances. Therefore, appropriate sample preparation methods, such as derivatization, liquid-liquid extraction, solid-phase extraction, solid-phase microextraction, and Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS), should be selected to remove the interferences and enrich target analytes before detection. The combination of effective sample preparation methods and appropriate instrument detection techniques is the key to determining the analysis efficiency and the result accuracy. To the best of our knowledge, there have been no review articles focused on sample preparation methods for the detection of furfural compounds in foods. Thus, this review aims to summarize the latest progress in sample preparation methods for furfural compound analysis in foods from 2012 to 2022. Their advantages and limitations are also discussed. The current review will help researchers choose suitable sample pretreatment and detection methods.
Sample preparation strategies for the analysis of contaminants in foods
2023, Innovation of Food Products in Halal Supply Chain Worldwide
Food safety standard is one of the critical aspects to ensure food safety and quality and is important for trade and consumer trust in halal products’ development. There is a demand for simple and reliable analysis of contaminants in foods to guarantee their safety and quality. The new strategies of sample preparation are moving toward more green and environmental friendly techniques, which use less sorbent and solvent and smaller sample sizes. This chapter aims to discuss the recent advances and applications of sample preparation techniques developed for different contaminants in foods, namely, liquid-phase microextraction, dispersive liquid–liquid microextraction, solid-phase microextraction, quick, easy, cheap, effective, rugged, safe, dispersive solid-phase extraction (SPE), and magnetic SPE. The principle and procedure, analytical figures of merit, level of contaminants found in the food matrices, and applicability of each technique in food analysis are discussed in detail.
Sample Preparation in Foodomics. Combination of Assisted-Extraction Techniques to the Comprehensive Foodomics
2020, Comprehensive Foodomics
International regulations regarding the presence of certain pollutants in foodstuffs demand new sample pre-treatment procedures and advanced instrumental techniques to assess very low concentrations of many sustances. In addition, foodstuffs are quite complex materials and interferences can arise from the major components such as large proteins, fats and carbohydrates. This chapter highlights the recent advances on coupling sorbent enrichment, liquid-phase, and membrane-based microextraction techniques for achieving efficient analyte extraction from foodstuff, as well as sequential/simultaneous target pre-concentration and/or extract clean-up. Several tandems involving microwave/ultrasound assisted extraction, pressurized fluid extraction, matrix solid phase dispersion, supercritical fluid extraction and quick, easy, cheap, effective, rugged and safe (QuEChERS) combined with sorbent-based and liquid-phase microextraction techniques for solid foodstuff have been reviewed. The state-of-the-art summary on current analytical parameters and methodological issues, such as enrichment factors, detection limits, and accuracy of the combined sample pre-treatment and the advantages and the limitations of current developments, and future prospects are discussed in details.
Contamination status of bisphenol A and its analogues (bisphenol S, F and B) in foodstuffs and the implications for dietary exposure on adult residents in Zhejiang Province
2019, Food Chemistry
An effective method has been developed for the simultaneous determination of four bisphenols (bisphenol A, S, F and B) in various foodstuffs. The contaminants were extracted by QuEChERS-based strategy and subjected to ion-exchange solid-phase extraction for further clean-up. The critical variables were screened by Plackett-Burman design and then optimized by central composite design. Under the optimized conditions, satisfactory accuracy (recoveries 76%–116%) and precision (RSDs < 12%) were achieved. The established method was then used to assess the contamination status of 379 real samples. Bisphenol A was demonstrated to be the predominant bisphenol with highest incidence (79.7%) and average concentration (14.3 μg/kg). The positive rates (mean concentration) of bisphenol S, F and B were 37.7% (1.6 μg/kg), 26.9% (1.4 μg/kg) and 0.0% (not detected), respectively. Finally, the daily dietary intakes of $\sum_{4} b i s p h e n o l s$ for adult residents were estimated (55.9–76.1 ng/kg bw/day) according to the contamination concentrations and the daily recommended intakes.
Combined assisted extraction techniques as green sample pre-treatments in food analysis
2019, TrAC - Trends in Analytical Chemistry
Citation Excerpt :
However, most of MAE applications involve aqueous solutions as extractants [19–29], and the addition of a solvent disperser is therefore needed for completing DLLME. Nitrosamines and polyamines [19–21], as well as polycyclic aromatic hydrocarbons (PAHs) [22–28] and veterinary residues [29] and phenolic compounds [30] have been commonly isolated from foodstuff by applying water/alcohol mixtures using potassium or sodium hydroxide for inducing hydrolyzation and saponification [19,20,22,23,25–27,29]. DLLME is applied after protein precipitation, and acetonitrile [21,26,27,29] and acetone [22–28] are mainly used as disperser solvents (methanol [19] and ethanol [20,30] have been also proposed).
This review highlights the increasing interest and application of combining sorbent enrichment, liquid-phase, and membrane-based microextraction techniques in Analytical Chemistry and its sustainable green applications to efficient target analyte extraction and pre-concentration/clean-up from foodstuff. Several combinings involving microwave/ultrasound assisted extraction, pressurised fluid extraction, matrix solid phase dispersion and supercritical fluid extraction and quick, easy, cheap, effective, rugged and safe (QuEChERS) combined with sorbent-based and liquid-phase microextraction techniques for solid foodstuff have been reviewed. The state-of-the-art summary on current analytical parameters and methodological issues, such as enrichment factors, detection limits, and accuracy of the combined sample pre-treatment and the advantages and the limitations of current developments, and future prospects were discussed in details.
Electrophoretic analysis of polyamines in exhaled breath condensate based on gold-nanoparticles microextraction coupled with field-amplified sample stacking
2019, Talanta
Citation Excerpt :
As shown in Table 1, Put and Cad showed good linearity over two orders of magnitudes (r > 0.999), and the LOD values could achieve 0.070–0.17 ng mL−1 (S/N = 3). Compared with most of the reported methods [8–13,15–23,25], this developed method could obtain comparable or higher detection sensitivity (LODs: 0.070–0.17 ng mL−1 vs 0.038–1000 ng mL−1) with no need of derivatization. ( The comparison table of analytical methods was listed in Table S2 of Supplementary file)
In this work, citrate-capped gold-nanoparticles (citrate-AuNPs) have been firstly used for selective extraction of trace polyamines, putrescine (Put) and cadaverine (Cad), followed by field-amplified sample stacking (FASS) coupled with capillary electrophoresis and capacitively coupled contactless conductivity detection (FASS-CE-C⁴D). Put and Cad were extracted by electrostatic attractions between the amine group of the polyamines and the citrate ligands adsorbed on the surfaces of AuNPs. AuNPs microextraction (AuNPs-ME) effectively shortened preparation time (50 min) by introducing ultrasound, and the required sample extraction volume was only 1 mL. Furthermore, a synergistic enrichment strategy based on off-line AuNPs-ME and on-line FASS significantly improved the detection sensitivity, making the enrichment factors up to 1726–1887 times. Under the optimum conditions, Put and Cad could be well separated from the potential coexisting substances and then directly determined by CE-C⁴D without derivatization. Due to its low sample consumption, high sensitivity (LODs: 0.070–0.17 ng mL⁻¹), and acceptable recoveries (90–105%), this AuNPs-ME/FASS-CE-C⁴D method provides a rapid, economical and eco-friendly approach for direct determination of polyamines in human exhaled breath condensate, and has potential application prospects in preliminary noninvasive diagnosis of oral and respiratory inflammation.

View all citing articles on Scopus

View full text

Application and optimization of microwave-assisted extraction and dispersive liquid–liquid microextraction followed by high-performance liquid chromatography for sensitive determination of polyamines in turkey breast meat samples

Highlights

Abstract

Introduction

Section snippets

Reagents, materials and standards

Results and discussion

Conclusion

Acknowledgment

Food Control

Microchemical Journal

Food Chemistry

Food Research International

Food Chemistry

Journal of Chromatography A

Journal of Chromatography A

Food Chemistry

Food Chemistry

Meat Science

Talanta

Journal of Chromatography B