Displaying publications 1 - 20 of 36 in total

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  1. A rapid MCM-41 dispersive micro-solid phase extraction coupled with LC/MS/MS for quantification of ketoconazole and voriconazole in biological fluids
    Yahaya N, Sanagi MM, Abd Aziz N, Wan Ibrahim WA, Nur H, Loh SH, et al.
    Biomed Chromatogr, 2017 Feb;31(2).
    PMID: 27474795 DOI: 10.1002/bmc.3803
    A rapid dispersive micro-solid phase extraction (D-μ-SPE) combined with LC/MS/MS method was developed and validated for the determination of ketoconazole and voriconazole in human urine and plasma samples. Synthesized mesoporous silica MCM-41 was used as sorbent in d-μ-SPE of the azole compounds from biological fluids. Important D-μ-SPE parameters, namely type desorption solvent, extraction time, sample pH, salt addition, desorption time, amount of sorbent and sample volume were optimized. Liquid chromatographic separations were carried out on a Zorbax SB-C18 column (2.1 × 100 mm, 3.5 μm), using a mobile phase of acetonitrile-0.05% formic acid in 5 mm ammonium acetate buffer (70:30, v/v). A triple quadrupole mass spectrometer with positive ionization mode was used for the determination of target analytes. Under the optimized conditions, the calibration curves showed good linearity in the range of 0.1-10,000 μg/L with satisfactory limit of detection (≤0.06 μg/L) and limit of quantitation (≤0.3 μg/L). The proposed method also showed acceptable intra- and inter-day precisions for ketoconazole and voriconazole from urine and human plasma with RSD ≤16.5% and good relative recoveries in the range 84.3-114.8%. The MCM-41-D-μ-SPE method proved to be rapid and simple and requires a small volume of organic solvent (200 μL); thus it is advantageous for routine drug analysis.
    Matched MeSH terms: Solid Phase Microextraction/economics; Solid Phase Microextraction/methods*
  2. A review of the modern principles and applications of solid-phase extraction techniques in chromatographic analysis
    Badawy MEI, El-Nouby MAM, Kimani PK, Lim LW, Rabea EI
    Anal Sci, 2022 Dec;38(12):1457-1487.
    PMID: 36198988 DOI: 10.1007/s44211-022-00190-8
    Analytical processes involving sample preparation, separation, and quantifying analytes in complex mixtures are indispensable in modern-day analysis. Each step is crucial to enriching correct and informative results. Therefore, sample preparation is the critical factor that determines both the accuracy and the time consumption of a sample analysis process. Recently, several promising sample preparation approaches have been made available with environmentally friendly technologies with high performance. As a result of its many advantages, solid-phase extraction (SPE) is practiced in many different fields in addition to the traditional methods. The SPE is an alternative method to liquid-liquid extraction (LLE), which eliminates several disadvantages, including many organic solvents, a lengthy operation time and numerous steps, potential sources of error, and high costs. SPE advanced sorbent technology reorients with various functions depending on the structure of extraction sorbents, including reversed-phase, normal-phase, cation exchange, anion exchange, and mixed-mode. In addition, the commercial SPE systems are disposable. Still, with the continual developments, the restricted access materials (RAM) and molecular imprinted polymers (MIP) are fabricated to be active reusable extraction cartridges. This review will discuss all the theoretical and practical principles of the SPE techniques, focusing on packing materials, different forms, and performing factors in recent and future advances. The information about novel methodological and instrumental solutions in relation to different variants of SPE techniques, solid-phase microextraction (SPME), in-tube solid-phase microextraction (IT-SPME), and magnetic solid-phase extraction (MSPE) is presented. The integration of SPE with analytical chromatographic techniques such as LC and GC is also indicated. Furthermore, the applications of these techniques are discussed in detail along with their advantages in analyzing pharmaceuticals, biological samples, natural compounds, pesticides, and environmental pollutants, as well as foods and beverages.
    Matched MeSH terms: Solid Phase Microextraction/methods
  3. Fulltext A study on volatile organic compounds emitted by in-vitro lung cancer cultured cells using gas sensor array and SPME-GCMS
    Thriumani R, Zakaria A, Hashim YZH, Jeffree AI, Helmy KM, Kamarudin LM, et al.
    BMC Cancer, 2018 04 02;18(1):362.
    PMID: 29609557 DOI: 10.1186/s12885-018-4235-7
    BACKGROUND: Volatile organic compounds (VOCs) emitted from exhaled breath from human bodies have been proven to be a useful source of information for early lung cancer diagnosis. To date, there are still arguable information on the production and origin of significant VOCs of cancer cells. Thus, this study aims to conduct in-vitro experiments involving related cell lines to verify the capability of VOCs in providing information of the cells.

    METHOD: The performances of e-nose technology with different statistical methods to determine the best classifier were conducted and discussed. The gas sensor study has been complemented using solid phase micro-extraction-gas chromatography mass spectrometry. For this purpose, the lung cancer cells (A549 and Calu-3) and control cell lines, breast cancer cell (MCF7) and non-cancerous lung cell (WI38VA13) were cultured in growth medium.

    RESULTS: This study successfully provided a list of possible volatile organic compounds that can be specific biomarkers for lung cancer, even at the 24th hour of cell growth. Also, the Linear Discriminant Analysis-based One versus All-Support Vector Machine classifier, is able to produce high performance in distinguishing lung cancer from breast cancer cells and normal lung cells.

    CONCLUSION: The findings in this work conclude that the specific VOC released from the cancer cells can act as the odour signature and potentially to be used as non-invasive screening of lung cancer using gas array sensor devices.

    Matched MeSH terms: Solid Phase Microextraction*
  4. Agarose- and alginate-based biopolymers for sample preparation: Excellent green extraction tools for this century
    Sanagi MM, Loh SH, Wan Ibrahim WN, Pourmand N, Salisu A, Wan Ibrahim WA, et al.
    J Sep Sci, 2016 Mar;39(6):1152-9.
    PMID: 27027592 DOI: 10.1002/jssc.201501207
    Recently, there has been considerable interest in the use of miniaturized sample preparation techniques before the chromatographic monitoring of the analytes in unknown complex compositions. The use of biopolymer-based sorbents in solid-phase microextraction techniques has achieved a good reputation. A great variety of polysaccharides can be extracted from marine plants or microorganisms. Seaweeds are the major sources of polysaccharides such as alginate, agar, agarose, as well as carrageenans. Agarose and alginate (green biopolymers) have been manipulated for different microextraction approaches. The present review is focused on the classification of biopolymer and their applications in multidisciplinary research. Besides, efforts have been made to discuss the state-of-the-art of the new microextraction techniques that utilize commercial biopolymer interfaces such as agarose in liquid-phase microextraction and solid-phase microextraction.
    Matched MeSH terms: Solid Phase Microextraction
  5. Agarose-chitosan-C18 film micro-solid phase extraction combined with high performance liquid chromatography for the determination of phenanthrene and pyrene in chrysanthemum tea samples
    Ng NT, Sanagi MM, Wan Ibrahim WN, Wan Ibrahim WA
    Food Chem, 2017 May 01;222:28-34.
    PMID: 28041555 DOI: 10.1016/j.foodchem.2016.11.147
    Agarose-chitosan-immobilized octadecylsilyl-silica (C18) film micro-solid phase extraction (μSPE) was developed and applied for the determination of phenanthrene (PHE) and pyrene (PYR) in chrysanthemum tea samples using high performance liquid chromatography-ultraviolet detection (HPLC-UV). The film of blended agarose and chitosan allows good dispersion of C18, prevents the leaching of C18 during application and enhances the film mechanical stability. Important μSPE parameters were optimized including amount of sorbent loading, extraction time, desorption solvent and desorption time. The matrix match calibration curves showed good linearity (r⩾0.994) over a concentration range of 1-500ppb. Under the optimized conditions, the proposed method showed good limits of detection (0.549-0.673ppb), good analyte recoveries (100.8-105.99%) and good reproducibilities (RSDs⩽13.53%, n=3) with preconcentration factors of 4 and 72 for PHE and PYR, respectively.
    Matched MeSH terms: Solid Phase Microextraction/methods*
  6. Fulltext Aphid-induced Defences in Chilli Affect Preferences of the Whitefly, Bemisia tabaci (Hemiptera: Aleyrodidae)
    Saad KA, Mohamad Roff MN, Hallett RH, Idris AB
    Sci Rep, 2015;5:13697.
    PMID: 26334135 DOI: 10.1038/srep13697
    The sweetpotato whitefly (WF), Bemisia tabaci, is a major pest that damages a wide range of vegetable crops in Malaysia. WF infestation is influenced by a variety of factors, including previous infestation of the host plant by other insect pests. This study investigated the effects of previous infestation of host chilli plants by the green peach aphid (Myzus persicae) on the olfactory behavioural response of B. tabaci, using free-choice bioassay with a Y-tube olfactometer. We analysed volatile organic compounds (VOCs) emitted by non-infested and M. persicae-infested chilli plants using solid-phase microextraction and gas chromatography-mass spectrometry. Our results showed that female WFs preferred non-infested to pre-infested plants. Collection and analysis of volatile compounds emitted by infested plants confirmed that there were significant increases in the production of monoterpenes (cymene; 1,8-cineole), sesquiterpenes (β-cadinene, α-copaene), and methyl salicylate (MeSA) compared to non-infested plants. Our results suggest that host plant infestation by aphids may induce production of secondary metabolites that deter B. tabaci from settling on its host plants. These results provide important information for understanding WF host selection and dispersal among crops, and also for manipulating WF behaviour to improve IPM in chilli.
    Matched MeSH terms: Solid Phase Microextraction
  7. Applications of solid-phase microextraction for the analysis of pesticide residues in fruits and vegetables: a review
    Abdulra'uf LB, Chai MK, Tan GH
    J AOAC Int, 2012 11 28;95(5):1272-90.
    PMID: 23175958
    This paper reviews the application of various modes of solid-phase microextraction (SPME) for the analysis of pesticide residues in fruits and vegetables. SPME is a simple extraction technique that eliminates the use of solvent, and it is applied for the analysis of both volatile and nonvolatile pesticides. SPME has been successfully coupled to both GC and LC. The coupling with GC has been straightforward and requires little modification of existing equipment, but interfacing with LC has proved challenging. The external standard calibration technique is widely used for quantification, while standard addition and internal or surrogate standards are mainly used to account for matrix effects. All parameters that affect the extraction of pesticide residues from fruits and vegetables, and therefore need to be optimized, are also reviewed. Details of the characteristics of analytical procedures and new trends in fiber production using sol-gel technology and molecularly imprinted polymers are discussed.
    Matched MeSH terms: Solid Phase Microextraction/methods*
  8. Assessment of dispersive liquid-liquid microextraction conditions for gas chromatography time-of-flight mass spectrometry identification of organic compounds in honey
    Moniruzzaman M, Rodríguez I, Rodríguez-Cabo T, Cela R, Sulaiman SA, Gan SH
    J Chromatogr A, 2014 Nov 14;1368:26-36.
    PMID: 25441341 DOI: 10.1016/j.chroma.2014.09.057
    The suitability of the dispersive liquid-liquid microextraction (DLLME) technique for gas chromatography (GC) characterization of minor organic compounds in honey samples is evaluated. Under optimized conditions, samples were pre-treated by liquid-liquid extraction with acetonitrile followed by DLLME using carbon tetrachloride (CCl4, 0.075 mL) as extractant. The yielded settled phase was analyzed by GC using high resolution time-of-flight (TOF) mass spectrometry (MS). The whole sample preparation process is completed in approximately 10 min, with a total consumption of organic solvents below 4 mL, relative standard deviations lower than 12% and with more than 70 organic compounds, displaying linear retention index in the range from 990 to 2900, identified in the obtained extracts. In comparison with HS SPME extraction, higher peak intensities were attained for most volatile and semi-volatile compounds amenable to both extraction techniques. Furthermore, other species such as highly polar and water soluble benzene acids, long chain fatty acids, esters and flavonoids, which are difficult to concentrate by HS SPME, could be identified in DLLME extracts. Some of the compounds identified in DLLME extracts have been proposed as useful for samples classification and/or they are recognized as markers of honeys from certain geographic areas.
    Matched MeSH terms: Solid Phase Microextraction
  9. Assessment of gas chromatography time-of-flight accurate mass spectrometry for identification of volatile and semi-volatile compounds in honey
    Moniruzzaman M, Rodríguez I, Ramil M, Cela R, Sulaiman SA, Gan SH
    Talanta, 2014 Nov;129:505-15.
    PMID: 25127626 DOI: 10.1016/j.talanta.2014.06.019
    The performance of gas chromatography (GC) combined with a hybrid quadrupole time-of-flight (QTOF) mass spectrometry (MS) system for the determination of volatile and semi-volatile compounds in honey samples is evaluated. After headspace (HS) solid-phase microextraction (SPME) of samples, the accurate mass capabilities of the above system were evaluated for compounds identification. Accurate scan electron impact (EI) MS spectra allowed discriminating compounds displaying the same nominal masses, but having different empirical formulae. Moreover, the use of a mass window with a width of 0.005 Da provided highly specific chromatograms for selected ions, avoiding the contribution of interferences to their peak areas. Additional information derived from positive chemical ionization (PCI) MS spectra and ion product scan MS/MS spectra permitted confirming the identity of novel compounds. The above possibilities are illustrated with examples of honey aroma compounds, belonging to different chemical classes and containing different elements in their molecules. Examples of compounds whose structures could not be described are also provided. Overall, 84 compounds, from a total of 89 species, could be identified in 19 honey samples from 3 different geographic areas in the world. The suitability of responses measured for selected ions, corresponding to above species, for authentication purposes is assessed through principal components analysis.
    Matched MeSH terms: Solid Phase Microextraction
  10. Characterisation of calamansi (Citrus microcarpa). Part II: volatiles, physicochemical properties and non-volatiles in the juice
    Cheong MW, Zhu D, Sng J, Liu SQ, Zhou W, Curran P, et al.
    Food Chem, 2012 Sep 15;134(2):696-703.
    PMID: 23107680 DOI: 10.1016/j.foodchem.2012.02.139
    Calamansi juices from three countries (Malaysia, the Philippines and Vietnam) were characterised through measuring volatiles, physicochemical properties and non-volatiles (sugars, organic acids and phenolic acids). The volatile components of manually squeezed calamansi juices were extracted using dichloromethane and headspace solid-phase microextraction, and then analysed using gas chromatography-mass spectrometry/flame ionisation detector, respectively. A total of 60 volatile compounds were identified. The results indicated that the Vietnam calamansi juice contained the highest amount of volatiles. Two principal components obtained from principal component analysis (PCA) represented 89.65% of the cumulative total variations of the volatiles. Among the non-volatile components, these three calamansi juices could be, to some extent, differentiated according to fructose and glucose concentrations. Hence, this study of calamansi juices could lead to a better understanding of calamansi fruits.
    Matched MeSH terms: Solid Phase Microextraction
  11. Characterization of a diesel-degrading strain isolated from a hydrocarbon-contaminated site
    Shukor MY, Dahalan FA, Jusoh AZ, Muse R, Shamaan NA, Syed MA
    J Environ Biol, 2009 Jan;30(1):145-50.
    PMID: 20112877
    A diesel-degrading bacterium has been isolated from a diesel-polluted site. The isolate was tentatively identified as Staphylococcus aureus strain DRY11 based on partial 16S rDNA molecular phylogeny and Biolog GP microplate panels and Microlog database. Isolate 11 showed an almost linear increase in cellular growth with respect to diesel concentrations with optimum growth occurring at 4% (v/v) diesel concentration. Optimization studies using different nitrogen sources showed that the best nitrogen source was potassium nitrite. Sodium nitrite was optimum at 1.2 g l(-1) and higher concentrations were strongly inhibitory to cellular growth. The optimal pH that supported growth of the bacterium was between 7.5 to 8.0 and the isolate exhibited optimal broad temperature supporting growth on diesel from 27 to 37 degrees C. An almost complete removal of diesel components was seen from the reduction in hydrocarbon peaks observed using Solid Phase Microextraction Gas Chromatography analysis after 5 days of incubation. The characteristics of this bacterium suggest that it is suitable for bioremediation of diesel spills and pollutions in the tropics.
    Matched MeSH terms: Solid Phase Microextraction
  12. Chemometric approach to the optimization of HS-SPME/GC-MS for the determination of multiclass pesticide residues in fruits and vegetables
    Abdulra'uf LB, Tan GH
    Food Chem, 2015 Jun 15;177:267-73.
    PMID: 25660885 DOI: 10.1016/j.foodchem.2015.01.031
    An HS-SPME method was developed using multivariate experimental designs, which was conducted in two stages. The significance of each factor was estimated using the Plackett-Burman (P-B) design, for the identification of significant factors, followed by the optimization of the significant factors using central composite design (CCD). The multivariate experiment involved the use of Minitab® statistical software for the generation of a 2(7-4) P-B design and CCD matrices. The method performance evaluated with internal standard calibration method produced good analytical figures of merit with linearity ranging from 1 to 500 μg/kg with correlation coefficient greater than 0.99, LOD and LOQ were found between 0.35 and 8.33 μg/kg and 1.15 and 27.76 μg/kg respectively. The average recovery was between 73% and 118% with relative standard deviation (RSD=1.5-14%) for all the investigated pesticides. The multivariate method helps to reduce optimization time and improve analytical throughput.
    Matched MeSH terms: Solid Phase Microextraction/methods*
  13. Fulltext Combination of Sensory, Chromatographic, and Chemometrics Analysis of Volatile Organic Compounds for the Discrimination of Authentic and Unauthentic Harumanis Mangoes
    Zakaria SR, Saim N, Osman R, Abdul Haiyee Z, Juahir H
    Molecules, 2018 Sep 16;23(9).
    PMID: 30223605 DOI: 10.3390/molecules23092365
    This study analyzed the volatile organic compounds (VOCs) of three mango varieties (Harumanis, Tong Dam and Susu) for the discrimination of authentic Harumanis from other mangoes. The VOCs of these mangoes were extracted and analysed nondestructively using Head Space-Solid Phase Micro Extraction (HS-SPME) coupled to Gas Chromatography-Mass Spectrometry (GC-MS). Prior to the analytical method, two simple sensory analyses were carried out to assess the ability of the consumers to differentiate between the Harumanis and Tong Dam mangoes as well as their preferences towards these mangoes. On the other hand, chemometrics techniques, such as principal components analysis (PCA), hierarchical clustering analysis (HCA), and discriminant analysis (DA), were used to visualise grouping tendencies of the volatile compounds detected. These techniques were successful in identifying the grouping tendencies of the mango samples according to the presence of their respective volatile compounds, thus enabling the identification of the groups of substances responsible for the discrimination between the authentic and unauthentic Harumanis mangoes. In addition, three ocimene compounds, namely beta-ocimene, trans beta-ocimene, and allo-ocimene, can be considered as chemical markers of the Harumanis mango, as these compounds exist in all Harumanis mango, regardless the different sources of the mangoes obtained.
    Matched MeSH terms: Solid Phase Microextraction
  14. Comparison of HS-SDME with SPME and SPE for the determination of eight organochlorine and organophosphorus pesticide residues in food matrices
    Kin CM, Huat TG
    J Chromatogr Sci, 2009 Sep;47(8):694-9.
    PMID: 19772747
    A headspace single-drop microextraction (HS-SDME) procedure is optimized for the analysis of organochlorine and organophosphorous pesticide residues in food matrices, namely cucumbers and strawberries by gas chromatography with an electron capture detector. The parameters affecting the HS-SDME performance, such as selection of the extraction solvent, solvent drop volume, extraction time, temperature, stirring rate, and ionic strength, were studied and optimized. Extraction was achieved by exposing 1.5 microL toluene drop to the headspace of a 5 mL aqueous solution in a 15-mL vial and stirred at 800 rpm. The analytical parameters, such as linearity, correlation coefficients, precision, limits of detection (LOD), limits of quantification (LOQ), and recovery, were compared with those obtained from headspace solid-phase microextraction (HS-SPME) and solid-phase extraction. The mean recoveries for all three methods were all above 70% and below 104%. HS-SPME was the best method with the lowest LOD and LOQ values. Overall, the proposed HS-SDME method is acceptable in the analysis of pesticide residues in food matrices.
    Matched MeSH terms: Solid Phase Microextraction/methods*
  15. Cyclodextrin based polymer sorbents for micro-solid phase extraction followed by liquid chromatography tandem mass spectrometry in determination of endogenous steroids
    Manaf NA, Saad B, Mohamed MH, Wilson LD, Latiff AA
    J Chromatogr A, 2018 Mar 30;1543:23-33.
    PMID: 29478831 DOI: 10.1016/j.chroma.2018.02.032
    Sorbents were prepared by cross-linking β-cyclodextrin (β-CD) using two different types of cross-linker units at variable reactant mole ratios. The resulting polymers containing β-CD were evaluated as sorbents in micro-solid phase extraction (μ-SPE) format for the extraction of the endogenous steroids testosterone (T), epitestosterone (E), androsterone (A), etiocholanolone (Etio), 5α-androstane-3α,17β-diol (5αAdiol) and 5β-androstane-3α,17β-diol (5βAdiol). The best sorbent (C1; cyclodextrin polymer) showed superior extraction characteristics compared with commercial sorbents (C18 and Bond Elut Plexa). Parameters influencing the extraction efficiency of the C1 sorbent such as extraction and desorption times, desorption solvent and volume of sample were investigated. The extracts were separated using a Hypersil Gold column (50 × 2.1 mm, 1.9 μm) under gradient elution coupled to a LC-MS/MS. The compounds were successfully separated within 8 min. The method offers good repeatability (RSD  0.995) were within the range of 1-200 ng mL-1 for T and E, 250-4000 ng mL-1 for A and Etio and 25-500 ng mL-1 for 5αAdiol and 5βAdiol, respectively. The method was applied for the determination of steroid profile of urine from volunteers.
    Matched MeSH terms: Solid Phase Microextraction*
  16. Effects of cucumber mosaic virus-infected chilli plants on non-vector Bemisia tabaci (Hemiptera: Aleyrodidae)
    Saad KA, Mohamad Roff MN, Hallett RH, Abd-Ghani IB
    Insect Sci, 2019 Feb;26(1):76-85.
    PMID: 28594105 DOI: 10.1111/1744-7917.12488
    Plant virus infections are known to alter host plant attractiveness and suitability for insect herbivores. This study was conducted to determine how cucumber mosaic virus (CMV)-infected chilli plants affect the fitness and settling preferences of nonvector whitefly, Bemisia tabaci adults under dual-choice conditions with volatile organic compounds analyzed using solid phase microextraction coupled with gas chromatography-mass spectrometry (GC-MS). Results showed that the presence of CMV in chilli plants substantially affects the settling preferences of the B. tabaci, which preferred to settle on noninfected plants. Duration of the egg stage and the longevity and fecundity of adult B. tabaci on CMV-infected chilli plants were not markedly different from those on noninfected chilli plants. In contrast, the developmental time from egg to adult was significantly reduced in CMV-infected chilli plants compared to the noninfected plants. The results also showed that CMV-infected chilli plants released significantly more linalool and phenylacetaldehyde than noninfected plants. Overall, it was suggested that the behavioral response of B. tabaci might be modified by CMV-infected plants, which alter the release of specific headspace volatiles. Based on these results, the modification of plant volatile profiles may help in enhancing the effectiveness of biological control and the protection of crop plants against B. tabaci.
    Matched MeSH terms: Solid Phase Microextraction
  17. Fulltext Headspace solid-phase microextraction gas chromatography-mass spectrometry and gas chromatography-olfactometry analysis of volatile compounds in pineapple breads
    Ying S, Lasekan O, Naidu KR, Lasekan S
    Molecules, 2012 Nov 22;17(12):13795-812.
    PMID: 23174897 DOI: 10.3390/molecules171213795
    Sensorial analysis of pineapple breads (conventionally baked, Cpb; fully baked frozen, Fpb and partially baked, Ppb) showed no significant differences in terms of aroma and taste. On the contrary, the scores for the overall quality between the partially baked and conventionally baked breads showed significant (p < 0.05) differences. At the same time, headspace analysis using a solid-phase microextraction (SPME) method identified 59 volatile compounds. The results of the aroma extracts dilution analysis (AEDA) revealed 19 most odour-active compounds with FD factors in the range of 32-128 as the key odourants of the pineapple breads. Further analysis of the similarities and differences between the pineapple breads in terms of the key odourants were carried out by the application of PLS-DA and PLS-regression coefficients. Results showed that Ppb exhibited strong positive correlations with most of the volatile- and non-volatile compounds, while the Cpb showed significant positive correlations with hexanal and 4-hydroxy-2,5-dimethyl-3(2H)-furanone, and the Fpb had strong positive correlations with lactic acid, benzoic acid, benzaldehyde and ethyl propanoate.
    Matched MeSH terms: Solid Phase Microextraction/methods*
  18. Headspace solid-phase microextraction gas chromatography-mass spectrometry determination of volatile compounds in different varieties of African star apple fruit (Chrysophillum albidum)
    Lasekan O, Khatib A, Juhari H, Patiram P, Lasekan S
    Food Chem, 2013 Dec 1;141(3):2089-97.
    PMID: 23870932 DOI: 10.1016/j.foodchem.2013.05.081
    The volatile compounds in four selected African star apple fruit (Chrysophyllum albidum) varieties were isolated and identified using the headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS). A total of 59 compounds were identified. Application of the aroma extract dilution analysis (AEDA) to the aroma distillates from the fruits revealed 45 odour-active compounds in the flavour dilution (FD) factor range of 4-128. Among them, the highest odour activities (FD factors) were determined for methylhexanoate, acetophenone and ethyl dodecanoate. Moreover, aroma lipophilicity appears to reflect molecular conformation. Further analysis of the similarities and differences between the fruit varieties in terms of the key odourants by the application of PLS-DA and PLS-regression coefficient showed strong positive correlation between the very sweet/sweet varieties and 10 key odourants. The odourants included ethyl acetate, acetyl methyl carbinol, methylhexanoate, sabinene, p-cymene, methylbenzoate, ethylbenzoate, geraniol, cis-α-bergomotene, acetophenone, and ethyl dodecanoate.
    Matched MeSH terms: Solid Phase Microextraction/instrumentation; Solid Phase Microextraction/methods*
  19. Hollow fiber liquid-phase microextraction coupled with gas chromatography-flame ionization detection for the profiling of fatty acids in vegetable oils
    Siang GH, Makahleh A, Saad B, Lim BP
    J Chromatogr A, 2010 Dec 24;1217(52):8073-8.
    PMID: 21081239 DOI: 10.1016/j.chroma.2010.10.052
    The development of a two phase hollow fiber liquid-phase microextraction technique, followed by gas-chromatography-flame ionization detection (GC-FID) for the profiling of the fatty acids (FAs) (lauric, myristic, palmitic, stearic, palmitoleic, oleic, linoleic, linolenic and arachidic) in vegetable oils is described. Heptadecanoic acid methyl ester was used as the internal standard. The FAs were transesterified to their corresponding methyl esters prior to the extraction. Extraction parameters such as type of extracting solvent, temperature, extraction time, stirring speed and salt addition were studied and optimized. Recommended conditions were extraction solvent, n-tridecane; extraction time, 35 min; extraction temperature, ambient; without addition of salt. Enrichment factors varying from 37 to 115 were achieved. Calibration curves for the nine FAs were well correlated (r(2)>0.994) within the range of 10-5000 μg L(-1). The limit of detection (signal:noise, 3) was 4.73-13.21 ng L(-1). The method was successfully applied to the profiling of the FAs in palm oils (crude, olein, kernel, and carotino cooking oil) and other vegetable oils (soybean, olive, coconut, rice bran and pumpkin). The encouraging enrichments achieved offer an interesting option for the profiling of the minor and major FAs in palm and other vegetable oils.
    Matched MeSH terms: Solid Phase Microextraction/methods*
  20. Magnetic poly(β-cyclodextrin-ionic liquid) nanocomposites for micro-solid phase extraction of selected polycyclic aromatic hydrocarbons in rice samples prior to GC-FID analysis
    Boon YH, Mohamad Zain NN, Mohamad S, Osman H, Raoov M
    Food Chem, 2019 Apr 25;278:322-332.
    PMID: 30583379 DOI: 10.1016/j.foodchem.2018.10.145
    Poly(β-cyclodextrin functionalized ionic liquid) immobilized magnetic nanoparticles (Fe3O4@βCD-Vinyl-TDI) as sorbent in magnetic µ-SPE was developed for the determination of selected polycyclic aromatic hydrocarbons (PAHs) in rice samples coupled with gas chromatographic-flame ionization detector (GC-FID). The nanocomposite was characterized by various tools and significant parameters that affected the extraction efficiency of PAHs were investigated. The calibration curves were linear for the concentration ranging between 0.1 and 500 μg kg-1 with correlation determinations (R2) from 0.9970 to 0.9982 for all analytes. Detection limits ranged at 0.01-0.18 μg kg-1 in real matrix. The RSD values ranged at 2.95%-5.34% (intra-day) and 4.37%-7.05% (inter-day) precision for six varied days. The sorbents showed satisfactory reproducibility in 2.9% to 9.9% range and acceptable recovery values at 80.4%-112.4% were obtained for the real sample analysis. The optimized method was successfully applied to access content safety of selected PAHs for 24 kinds of commercial rice available in Malaysia.
    Matched MeSH terms: Solid Phase Microextraction/instrumentation; Solid Phase Microextraction/methods*
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