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Novel solid-phase membrane tip extraction and gas chromatography with mass spectrometry methods for the rapid analysis of triazine herbicides in real waters

Sanagi MM, Muhammad SS, Hussain I, Ibrahim WA, Ali I

J Sep Sci, 2015 Feb;38(3):433-8.
PMID: 25421899 DOI: 10.1002/jssc.201400912

Novel, fast, selective, eco-friendly and reproducible solid-phase membrane tip extraction and gas chromatography with mass spectrometry methods were developed and validated for the analysis of triazine herbicides (atrazine and secbumeton) in stream and lake waters. The retention times of atrazine and secbumeton were 7.48 and 8.51 min. The solid-phase membrane tip extraction was carried out in semiautomated dynamic mode on multiwall carbon nanotubes enclosed in a cone-shaped polypropylene membrane cartridge. Acetone and methanol were found as the best preconditioning and desorption solvents, respectively. The extraction and desorption times for these herbicides were 15.0 and 10.0 min, respectively. The percentage recoveries of atrazine and secbumeton were 88.0 and 99.0%. The linearity range was 0.50-80.0 μg/L (r(2) > 0.994), with detection limits (<0.47 μg/L, S/N = 3) and good reproducibility (<8.0%). The ease of operation, eco-friendly nature, and low cost of solid-phase membrane tip extraction made these methods novel. The Solid-phase membrane tip extraction method was optimized by considering the effect of extraction time, desorbing solvents and time.

Matched MeSH terms: Solid Phase Extraction
Phenylethanoid glycosides isolated from Paraboea paniculata

Yue TH, Hock AH, Kiang LC, Mooi LY

Nat Prod Commun, 2012 Jun;7(6):775-8.
PMID: 22816305

Phytochemical studies of the leaves and rhizomes of Paraboea pa niculata (Gesneriaceae) are reported for the first time. Three phenylethanoid glycosides were isolated and characterized as 3,4-dihydroxyphenethyl-(3"-O-beta-D-apiofuranosyl)-beta-D-glucopyranoside, calceoralarioside E, and acteoside. These isolates exhibited weak cytotoxic activity against the K-562 cell line with a 50% of cell killing rate of 40.18 microM, 27.05 microM, and 27.24 microM, respectively. In the DPPH free radical scavenging assay, their IC50 values were determined as 75.89 microM, 25.00 microM, and 26.04 microM, respectively.

Matched MeSH terms: Solid Phase Extraction
Low temperature followed by matrix solid-phase dispersion-sonication procedure for the determination of multiclass pesticides in palm oil using LC-TOF-MS

Sobhanzadeh E, Abu Bakar NK, Bin Abas MR, Nemati K

J Hazard Mater, 2011 Feb 28;186(2-3):1308-13.
PMID: 21177032 DOI: 10.1016/j.jhazmat.2010.12.001

A simple and effective multiresidue method based on precipitation at low temperature followed by matrix solid-phase dispersion-sonication was developed and validated to determine dimethoate, malathion, carbaryl, simazine, terbuthylazine, atrazine and diuron in palm oil using liquid chromatography time-of-flight mass spectrometry (LC-TOF-MS). Liquid-liquid extraction (LLE) followed by low temperature method were optimized by studying the effect of type and volume of organic solvent (acetonitrile, acetonitrile:n-hexane (3:2 v/v) and acetone) and time of freezing to obtain high recovery yield and low co-extract fat residue in the final extract. The optimal conditions for matrix solid-phase dispersion (MSPD) were obtained using 5 g of palm oil, 2 g of primary secondary amine (PSA) as dispersing sorbent, 1 g of graphitized carbon black (GCB) as clean-up sorbent and 15 mL of acetonitrile as eluting solvent under conditions of 15 min ultrasonication at room temperature. Method validation was performed in order to study sensitivity, linearity, precision, and accuracy. Average recoveries at three concentration levels (25, 50 and 100 μg kg(-1)) were found in the range of 72.6-91.3% with relative standard deviations between 5.3% and 14.2%. Detection and quantification limits ranged from 1.5 to 5 μg kg(-1) and from 2.5 to 9 μg kg(-1), respectively.

Matched MeSH terms: Solid Phase Extraction
Analysis of selected pesticides and alkylphenols in human cord blood by gas chromatograph-mass spectrometer

Tan BL, Ali Mohd M

Talanta, 2003 Nov 4;61(3):385-91.
PMID: 18969198 DOI: 10.1016/S0039-9140(03)00281-9

A total of seven pesticides and eight alkylphenols were monitored using this method for the determination of their trace levels in human cord blood. The pesticides are lindane, diazinon, alpha-endosulfan, beta-endosulfan, endosulfan sulfate, chlorpyrifos and endrin; while the alkylphenols are 4-n-butylphenol, 4-n-pentylphenol, 4-n-hexylphenol, 4-t-octylphenol, 4-n-heptylphenol, nonylphenol, 4-n-octylphenol and bisphenol A. The pesticides and alkylphenols in the cord blood samples were extracted with solid phase extraction IST C18 cartridges and analyzed by selected ion monitoring mode using quadrapole detector in Shimadzu QP-5000 gas chromatograph-mass spectrometer. Trace levels of pesticide and alkylphenols in the range of non-detectable to 15.17 ng ml(-1), were detected in the human cord blood samples. This technique of monitoring the levels of endocrine-disruptors in blood samples is consistent, reliable and cost effective while reducing wastage of time and solvents.

Matched MeSH terms: Solid Phase Extraction
High Throughput Residue Analysis of Indaziflam and its Metabolites in Palm Oil Using Liquid Chromatography-Tandem Mass Spectrometry

Halim N, Kuntom A, Shinde R, Banerjee K

J AOAC Int, 2020 Sep 01;103(5):1237-1242.
PMID: 33241391 DOI: 10.1093/jaoacint/qsaa041

BACKGROUND: Indaziflam (IND) is a herbicide that is used in palm oil plantations for broad spectrum management of weeds. Until now, no validated method has been available for residue estimation of this herbicide in palm oil products.
OBJECTIVE: In this study, we report a rapid method for the residue analysis of IND and its metabolites, viz., IND-carboxylic acid, diaminotriazine, and triazine indanone in a wide range of palm oil matrices using liquid chromatography-tandem mass spectrometry (LC-MS/MS).
METHOD: The optimized sample preparation workflows included two options: (1) acetonitrile extraction (QuEChERS workflow), followed by freezing at -80°C and (2) acetonitrile extraction, followed by cleanup through a C18 solid phase extraction (SPE) cartridge. The optimized LC runtime was 7 min. All these analytes were estimated by LC-MS/MS multiple reaction monitoring.
RESULTS: Both sample preparation methods provided similar method performance and acceptable results. The limit of quantification (LOQ) of IND, IND-carboxylic acid, and triazine indanone was 0.001 mg/kg. For diaminotriazine, the LOQ was 0.005 mg/kg. The method accuracy and precision complied with the SANTE/12682/2019 guidelines of analytical quality control.
CONCLUSIONS: The potentiality of the method lies in a high throughput analysis of IND and its metabolites in a single chromatographic run with high selectivity and sensitivity. Considering its fit-for-purpose performance, the method can be implemented in regulatory testing of IND residues in a wide range of palm oil matrices that are consumed and traded worldwide.
HIGHLIGHTS: This work has provided a validated method for simultaneous residue analysis of indaziflam and its metabolites in crude palm oil and its derived matrices with high sensitivity, selectivity, and throughput.

Matched MeSH terms: Solid Phase Extraction
Fulltext Physicochemical properties and water quality parameter of paddy soil and water and their relationship with pesticides concentration

Siti Zulfa Zaidon, Yu Bin Ho, Zailina Hashim, Nazamid Saari, Sarva Mangala Praveena

Malaysian Journal of Medicine and Health Sciences, 2020;16(2):206-214.
MyJurnal

Introduction: Pesticides may influence the physicochemical properties of soil and the water quality parameters, which is vital in maintaining soil fertility and producing high quality crops. Objective: This study aims to determine the relationship between the concentration of pesticides, the physicochemical properties of the paddy soil samples and the water quality parameters of paddy water samples. Methods: A total of 72 soil and 72 water samples were collected in Tanjung Karang, Malaysia. The paddy soil and water were extracted using Quick, Easy, Cheap, Efficient, Rugged and Safe (QuEChERS) and solid phase extraction (SPE) techniques respectively. The concentrations of pesti- cides were analysed in ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). The relationship of the concentration of target pesticides and the paddy soil and water physicochemical properties were studied using Spearman correlation. Results: In paddy soil, the concentration of propiconazole shows moderate positive correlation with manganese (Mn) (r = 0.587) (p 0.01). Meanwhile buprofezin-total organic carbon (TOC) (r = -0.55) (p 0.01), imidacloprid-cation exchange capacity (CEC) (r = -0.519) (p 0.01), pymetrozine-sodium (Na) (r = -0.588) (p 0.01), and trifloxystrobin-calcium (Ca) (r = 0.566) (p 0.01) showed moderate negative correlation. Whereas in water, trifloxystrobin showed significant positive correlation with turbidity (r = 0.718) (p 0.01) and te- buconazole showed negative correlation to dissolved oxygen (DO) (r = 0.634) (p 0.01). Conclusion: The presence of pesticides in paddy field may influence the soil and water quality, thus regular monitoring of pesticides usage and nutrient management in soil is deemed important.

Matched MeSH terms: Solid Phase Extraction
Cellulose supported promising magnetic sorbents for magnetic solid-phase extraction: A review

Mhd Haniffa MAC, Ching YC, Illias HA, Munawar K, Ibrahim S, Nguyen DH, et al.

Carbohydr Polym, 2021 Feb 01;253:117245.
PMID: 33279000 DOI: 10.1016/j.carbpol.2020.117245

Cellulose with ample hydroxyl groups is considered as a promising supportive biopolymer for fabricating cellulose supported promising magnetic sorbents (CMS) for magnetic solid-phase extraction (MSPE). The easy recovery via external magnetic field, and recyclability of CMS, associated with different types and surface modifications of cellulose has made them a promising sorbent in the field of solid-phase extraction. CMS based sorbent can offer improved adsorption and absorption capabilities due to its high specific surface area, porous structure, and magnetic attraction feature. This review mainly focuses on the fabrication strategies of CMS using magnetic nanoparticles (MNPs) and various forms of cellulose as a heterogeneous and homogeneous solution either in alkaline mediated urea or Ionic liquids (ILs). Moreover, CMS will be elaborated based on their structures, synthesis, physical performance, and chemical attraction of MNPs and their MSPE in details. The advantages, challenges, and prospects of CMS in future applications are also presented.

Matched MeSH terms: Solid Phase Extraction
Magnetized graphene layers synthesized on the carbon nanofibers as novel adsorbent for the extraction of polycyclic aromatic hydrocarbons from environmental water samples

Rezvani-Eivari M, Amiri A, Baghayeri M, Ghaemi F

J Chromatogr A, 2016 Aug 16.
PMID: 27578405 DOI: 10.1016/j.chroma.2016.08.034

The application of magnetized graphene (G) layers synthesized on the carbon nanofibers (CNFs) (m-G/CNF) was investigated as novel adsorbent for the magnetic solid-phase extraction (MSPE) of polycyclic aromatic hydrocarbons (PAHs) in water samples followed by gas chromatography-flame ionization detector (GC-FID). Six important parameters, affecting the extraction efficiency of PAHs, including: amount of adsorbent, adsorption and desorption times, type and volume of the eluent solvent and salt content of the sample were evaluated. The optimum extraction conditions were obtained as: 5min for extraction time, 20mg for sorbent amount, dichloromethane as desorption solvent, 1mL for desorption solvent volume, 5min for desorption time and 15% (w/v) for NaCl concentration. Good performance data were obtained at the optimized conditions. The calibration curves were linear over the concentration ranges from 0.012 to 100ngmL(-1) with correlation coefficients (r) between 0.9950 and 0.9967 for all the analytes. The limits of detection (LODs, S/N=3) of the proposed method for the studied PAHs were 0.004-0.03ngmL(-1). The relative standard deviations (RSDs) for five replicates at two concentration levels (0.1 and 50ngmL(-1)) of PAHs were ranged from 3.4 to 5.7%. Appropriate relative recovery values, in the range of 95.5-99.9%, were also obtained for the real water sample analysis.

Matched MeSH terms: Solid Phase Extraction
Dispersive liquid-liquid microextraction combined with dispersive solid-phase extraction for gas chromatography with mass spectrometry determination of polycyclic aromatic hydrocarbons in aqueous matrices

Mohd Hassan FW, Muggundha Raoov, Kamaruzaman S, Sanagi MM, Yoshida N, Hirota Y, et al.

J Sep Sci, 2018 Oct;41(19):3751-3763.
PMID: 30125466 DOI: 10.1002/jssc.201800326

This study describes a dispersive liquid-liquid microextraction combined with dispersive solid-phase extraction method based on phenyl-functionalized magnetic sorbent for the preconcentration of polycyclic aromatic hydrocarbons from environmental water, sugarcane juice, and tea samples prior to gas chromatography with mass spectrometry analysis. Several important parameters affecting the extraction efficiency were investigated thoroughly, including the mass of sorbent, type and volume of extraction solvent, extraction time, type of desorption solvent, desorption time, type and amount of salt-induced demulsifier, and sample volume. Under the optimized extraction and gas chromatography-mass spectrometric conditions, the method revealed good linearity (10-100000 ng/L) with coefficient of determination (R2 ) of ≥0.9951, low limits of detection (3-16 ng/L), high enrichment factors (61-239), and satisfactory analyte recoveries (86.3-109.1%) with the relative standard deviations

Matched MeSH terms: Solid Phase Extraction
Fulltext Release of bisphenol a from polycarbonate and polyethylene terephthalate drinking water bottles under different storage conditions and its associated health risk

Wen Min Yun, Yu Bin Ho, Eugenie Sin Sing Tan, Vivien How

Malaysian Journal of Medicine and Health Sciences, 2018;14(102):1-9.
MyJurnal

Bisphenol A (BPA) is a controversial plastics ingredient used mainly in the production of polycarbonate plastics (PC) and epoxy resins that widely used nowadays in food and drink packaging. Even though BPA is not involved in polyethylene terephthalate (PET) manufacturing, recent study had reported the present of BPA in PET water bottle. This study was conducted to investigate effects storage conditions on release of BPA from PC and PET bottled water as well as to assess health risks associated with consumption. Methods: Solid phase extraction (SPE) was used to extract the samples, followed by analysis using ultra high performance liquid chromatography with fluorescence detector (UHPLC-FLD). The possibility of developing chronic non-carcinogenic health risk among consumers of bottled water was evaluated using hazard quotient (HQ). Results: Results showed that BPA migrated from PC and PET water bottles at concentrations ranging from 9.13 to 257.67 ng/L and 11.53 ng/L to 269.87 ng/L respectively. Concentrations of BPA were higher in PET bottled water compared to PC bottled water across all storage conditions. Higher storage temperature and longer storage duration increased BPA concentrations in PC and PET bottled water. Concentrations of BPA in bottled water which were kept in a car and were exposed to sunlight were higher than control samples which were stored indoor at room temperature. Conclusion: No significant chronic non-carcinogenic health risks were calculated for daily ingestion of BPA-contaminated bottled water; calculated HQ was less than one.

Matched MeSH terms: Solid Phase Extraction
Fulltext Synthesis, Characterization, and Application of Poly(4,4'-Cyclohexylidene Bisphenol Oxalate) for Solid-Phase Extraction of DNA

Al Balawi AN, Yusof NA, Kamaruzaman S, Mohammad F, Wasoh H, Al Abbosh KF, et al.

Biomed Res Int, 2019;2019:7064073.
PMID: 30868072 DOI: 10.1155/2019/7064073

The present study has synthesized poly(4,4'-cyclohexylidene bisphenol oxalate) by the condensation of oxalyl chloride with 4,4'-cyclohexylidene bisphenol, where its efficacy was tested for the solid-phase extraction of DNA. The synthesized polymer in the form of a white powder was characterized by FTIR, TGA-DTG, SEM, and BET analysis. The study utilized solid-phase application of the resulting polymer to extract DNA. The analysis of results provided the information that the extraction efficiency is a strong dependent of polymer amount and binding buffer type. Among the three types of buffers tested, the GuHCl buffer produced the most satisfactory results in terms of yield and efficiency of extraction. Moreover, the absorbance ratio of A260/A280 in all of the samples varied from 1.682 to 1.491, thereby confirming the capability of poly(4,4'-cyclohexylidene bisphenol oxalate) to elute pure DNA. The results demonstrated an increased DNA binding capacity with respect to increased percentage of the polymer. The study has concluded that poly(bisphenol Z oxalate) can be applied as one of the potential candidates for the high efficiency extraction of DNA by means of a simple, cost-effective, and environmentally friendly approach compared to the other traditional solid-phase methods.

Matched MeSH terms: Solid Phase Extraction
Detection of gliclazide in aqueous samples using liquid chromatography/time-of-flight/mass spectrometry

Fouad Fadhil Al-Qaim, Md Pauzi Abdullah, Jalifah Latip, Wan Mohd Afiq Wan Mohd Khalik, Nurfaizah Abu Tahrim, Nurul Auni Zainal Abidin, et al.

Sains Malaysiana, 2016;45:803-810.

The big challenge for the detection of pharmaceutical residues in water samples is the type of ionization mode in
terms of positive or negative ionization which plays an important role to identify and quantify the analytes using liquid
chromatography/mass spectrometry. An analytical method was applied to analysis of gliclazide (diabetic drug) in surface
water and wastewater from sewage treatment plants and hospitals. The proposed analytical method allows simultaneous
isolation and concentration procedure using solid phase extraction (Oasis HLB) prior to separation using high-performance
liquid chromatography. The detection and confirmation was achieved by applying time-of-flight analyzer. The limits of
quantification were as low as 1.4 ng/L (deionized water), 4 ng/L (surface water), 27 ng/L (hospital influent), 10 ng/L
(hospital effluent), 6 ng/L (sewage treatment plant effluent) and 21 ng/L (sewage treatment plant influent), respectively. On
average, good recoveries of higher than 87% were obtained for gliclazide in the studied samples. The proposed method
successfully determined and quantified gliclazide in surface water and wastewater. The results showed that gliclazide
is a persistent compound in sewage treatment effluents as well as in the recipient rivers. Gliclazide was detected in all
samples and the highest concentration was 130 ng/L in influent of sewage treatment plant.

Matched MeSH terms: Solid Phase Extraction
Pharmaceuticals, hormones, plasticizers, and pesticides in drinking water

Wee SY, Ismail NAH, Haron DEM, Yusoff FM, Praveena SM, Aris AZ

J Hazard Mater, 2022 02 15;424(Pt A):127327.
PMID: 34600377 DOI: 10.1016/j.jhazmat.2021.127327

Humans are exposed to endocrine disrupting compounds (EDCs) in tap water via drinking water. Currently, most of the analytical methods used to assess a long list of EDCs in drinking water have been made available only for a single group of EDCs and their metabolites, in contrast with other environmental matrices (e.g., surface water, sediments, and biota) for which more robust methods have been developed that allow detection of multiple groups. This study reveals an analytical method of one-step solid phase extraction, incorporated together with liquid chromatography-tandem mass spectrometry for the quantification of multiclass EDCs (i.e., pharmaceuticals, hormones, plasticizers, and pesticides) in drinking water. Fifteen multiclass EDCs significantly varied in amount between field samples (p

Matched MeSH terms: Solid Phase Extraction
Polyaniline-dicationic ionic liquid coated with magnetic nanoparticles composite for magnetic solid phase extraction of polycyclic aromatic hydrocarbons in environmental samples

Shahriman MS, Ramachandran MR, Zain NNM, Mohamad S, Manan NSA, Yaman SM

Talanta, 2018 Feb 01;178:211-221.
PMID: 29136814 DOI: 10.1016/j.talanta.2017.09.023

In this present study, magnetic nanoparticles (MNPs) nanocomposites modified with polyaniline (PANI) coated newly synthesised dicationic ionic liquid (DICAT) forming MNP-PANI-DICAT were successfully synthesised as new generation material for magnetic solid phase extraction (MSPE). MNP-PANI-DICAT was characterised by FT-IR NMR, CHN, BET, SEM, TEM, and VSM techniques and the results were compared with MNP-PANI and native MNP. This new material was applied as a magnetic adsorbent for the pre-concentration and separation of polycyclic aromatic hydrocarbons (PAHs) due to the π-π interaction between polyaniline shell and dicationic ionic liquid (DICAT) with PAHs compounds. Under the optimal conditions, the proposed method was evaluated and applied for the analysis of PAHs in environmental samples using gas chromatography-mass spectrometry (GC-MS). The validation method showed good linearity (0.005-500µgL-1) with the coefficient of determination (R2) > 0.999. The limits of detection (LOD) and quantification (LOQ) of the developed method (MNP-PANI-DICAT-MSPE) were in the range of 0.0008-0.2086µgL-1and 0.0024-0.6320µgL-1, respectively. The enrichment factor (EF) of PAHs on MNP-PANI-DICAT-MSPE were in the range of 7.546-29.632. The extraction recoveries of natural water, sludge, and soil samples were ranged from 80.2% to 111.9% with relative standard deviation (RSD) less than 5.6%. The newly synthesised MNP-PANI-DICAT possess good sensitivity, reusability, and fast extraction of PAHs under the MSPE procedure in various environmental samples.

Matched MeSH terms: Solid Phase Extraction
Fulltext Anticoagulant Activity of Polyphenolic-Polysaccharides Isolated from Melastoma malabathricum L

Khoo LT, Abas F, Abdullah JO, Mohd Tohit ER, Hamid M

Evid Based Complement Alternat Med, 2014;2014:614273.
PMID: 24987430 DOI: 10.1155/2014/614273

Melastoma malabathricum Linn. is a perennial traditional medicine plants that grows abundantly throughout Asian countries. In this study, M. malabathricum Linn. leaf hot water crude extract with anticoagulant activity was purified through solid phase extraction cartridge and examined for the bioactive chemical constituents on blood coagulation reaction. The SPE purified fractions were, respectively, designated as F1, F2, F3, and F4, and each was subjected to the activated partial thromboplastin time (APTT) anticoagulant assay. Active anticoagulant fractions (F1, F2, and F3) were subjected to chemical characterisation evaluation. Besides, neutral sugar for carbohydrate part was also examined. F1, F2, and F3 were found to significantly prolong the anticoagulant activities in the following order, F1 > F2 > F3, in a dose dependent manner. In addition, carbohydrate, hexuronic acid, and polyphenolic moiety were measured for the active anticoagulant fractions (F1, F2, and F3). The characterisation of chemical constituents revealed that all these three fractions contained acidic polysaccharides (rhamnogalacturonan, homogalacturonan, and rhamnose hexose-pectic type polysaccharide) and polyphenolics. Hence, it was concluded that the presence of high hexuronic acids and polysaccharides, as well as polyphenolics in traditional medicinal plant, M. malabathricum, played a role in prolonging blood clotting in the intrinsic pathway.

Matched MeSH terms: Solid Phase Extraction
Fulltext Influence of conventional and ultrasonic-assisted extraction on phenolic contents, betacyanin contents, and antioxidant capacity of red dragon fruit (Hylocereus polyrhizus)

Ramli NS, Ismail P, Rahmat A

ScientificWorldJournal, 2014;2014:964731.
PMID: 25379555 DOI: 10.1155/2014/964731

The aim of this study was to examine the effects of extraction methods on antioxidant capacities of red dragon fruit peel and flesh. Antioxidant capacities were measured using ethylenebenzothiozoline-6-sulfonic acid (ABTS) radical cation assay and ferric reducing antioxidant power assay (FRAP). Total phenolic content (TPC) was determined using Folin-Ciocalteu reagent while quantitative determination of total flavonoid content (TFC) was conducted using aluminium trichloride colorimetric method. Betacyanin content (BC) was measured by spectrophotometer. Red dragon fruit was extracted using conventional (CV) and ultrasonic-assisted extraction (UE) technique to determine the most efficient way of extracting its antioxidant components. Results indicated that UE increased TFC, reduced the extraction yield, BC, and TPC, but exhibited the strongest scavenging activity for the peel of red dragon fruit. In contrast, UE reduced BC, TFC, and scavenging activity but increased the yield for the flesh. Nonetheless, UE slightly increases TPC in flesh. Scavenging activity and reducing power were highly correlated with phenolic and flavonoid compounds. Conversely, the scavenging activity and reducing power were weakly correlated with betacyanin content. This work gives scientific evidences for the consideration of the type of extraction techniques for the peel and flesh of red dragon fruit in applied research and food industry.

Matched MeSH terms: Solid Phase Extraction/methods
Multi-residue analytical methodology-based liquid chromatography-time-of-flight-mass spectrometry for the analysis of pharmaceutical residues in surface water and effluents from sewage treatment plants and hospitals

Al-Qaim FF, Abdullah MP, Othman MR, Latip J, Zakaria Z

J Chromatogr A, 2014 Jun 6;1345:139-53.
PMID: 24768127 DOI: 10.1016/j.chroma.2014.04.025

An analytical method that facilitated the analysis of 11 pharmaceuticals residue (caffeine, prazosin, enalapril, carbamazepine, nifedipine, levonorgestrel, simvastatin, hydrochlorothiazide, gliclazide, diclofenac-Na, and mefenamic acid) with a single pre-treatment protocol was developed. The proposed method included an isolation and concentration procedure using solid phase extraction (Oasis HLB), a separation step using high-performance liquid chromatography, and a detection procedure that applies time-of-flight mass spectrometry. The method was validated for drinking water (DW), surface water (SW), sewage treatment plant (STP) influent and effluent, and hospital (HSP) influent and effluent. The limits of quantification were as low as 0.4, 1.6, 5, 3, 2.2 and 11 ng/L in DW, SW, HSP influent and effluent, STP effluent, and STP influent, respectively. On average, good recoveries higher than 75% were obtained for most of the target analytes in all matrices. Matrix effect was evaluated for all samples matrices. The proposed method successfully determined and quantified the target compounds in raw and treated wastewater of four STPs and three hospitals in Malaysia, as well as in two SW sites. The results showed that a number of the studied compounds pose moderate to high persistency in sewage treatment effluents as well as in the recipient rivers, namely; caffeine, simvastatin, and hydrochlorothiazide. Ten out of 11 compounds were detected and quantified in 13 sampling points. Caffeine was detected with the highest level, with concentrations reaching up to 9099 ng/L in STP influent.

Matched MeSH terms: Solid Phase Extraction/methods
Determination of polar aromatic amines using newly synthesized sol-gel titanium (IV) butoxide cyanopropyltriethoxysilane as solid phase extraction sorbent

Miskam M, Abu Bakar NK, Mohamad S

Talanta, 2014 Mar;120:450-5.
PMID: 24468395 DOI: 10.1016/j.talanta.2013.12.037

A solid phase extraction (SPE) method has been developed using a newly synthesized titanium (IV) butoxide-cyanopropyltriethoxysilane (Ti-CNPrTEOS) sorbent for polar selective extraction of aromatic amines in river water sample. The effect of different parameters on the extraction recovery was studied using the SPE method. The applicability of the sorbents for the extraction of polar aromatic amines by the SPE was extensively studied and evaluated as a function of pH, conditioning solvent, sample loading volume, elution solvent and elution solvent volume. The optimum experimental conditions were sample at pH 7, dichloromethane as conditioning solvent, 10 mL sample loading volume and 5 mL of acetonitrile as the eluting solvent. Under the optimum conditions, the limit of detection (LOD) and limit of quantification (LOQ) for solid phase extraction using Ti-CNPrTEOS SPE sorbent (0.01-0.2; 0.03-0.61 µg L(-1)) were lower compared with those achieved using Si-CN SPE sorbent (0.25-1.50; 1.96-3.59 µg L(-1)) and C18 SPE sorbent (0.37-0.98; 1.87-2.87 µg L(-1)) with higher selectivity towards the extraction of polar aromatic amines. The optimized procedure was successfully applied for the solid phase extraction method of selected aromatic amines in river water, waste water and tap water samples prior to the gas chromatography-flame ionization detector separation.

Matched MeSH terms: Solid Phase Extraction/methods*
Novel sol-gel hybrid methyltrimethoxysilane-tetraethoxysilane as solid phase extraction sorbent for organophosphorus pesticides

Wan Ibrahim WA, Veloo KV, Sanagi MM

J Chromatogr A, 2012 Mar 16;1229:55-62.
PMID: 22326188 DOI: 10.1016/j.chroma.2012.01.022

A novel sol-gel hybrid methyltrimethoxysilane-tetraethoxysilane (MTMOS-TEOS) was produced and applied as sorbent for solid phase extraction (SPE). Five selected organophosphorus pesticides (OPPs) were employed as model compounds to evaluate the extraction performance of the synthesized sol-gel organic-inorganic hybrid MTMOS-TEOS. Analysis was performed using gas chromatography-mass spectrometry. Several important SPE parameters were optimized. Under the optimum extraction conditions, the method using the sol-gel organic-inorganic hybrid MTMOS-TEOS as SPE sorbent showed good linearity in the range of 0.001-1 μg L(-1), good repeatability (RSD 2.1-3.1%, n=5), low limits of detection at S/N=3 (0.5-0.9 pg mL(-1)) and limit of quantification (1-3 pg mL(-1), S/N=10). The performance of the MTMOS-TEOS SPE was compared to commercial C18 Supelclean SPE since C18 SPE is widely used for OPPs. The MTMOS-TEOS SPE method LOD was 500-600 × lower than the LOD of commercial C18 SPE. The LOD achieved with the sol-gel organic-inorganic hybrid MTMOS-TEOS SPE sorbent allowed the detection of these OPPs in drinking water well below the level set by European Union (EU) at 0.1 μg L(-1) of each pesticides. The developed MTMOS-TEOS SPE method was successfully applied to real sample analysis of the selected OPPs from several water samples and its application extended to the analysis of several fruits samples. Excellent recoveries and RSDs of the OPPs were obtained from the various water samples (recoveries: 97-111%, RSDs 0.4-2.8%, n=3) and fruit samples (recoveries: 96-111%), RSDs 1-4%, n=5) using the sol-gel organic-inorganic hybrid MTMOS-TEOS SPE sorbent. Recoveries and RSDs of OPPs from river water samples and fruit samples using C18 Supelclean SPE sorbent were 91-97%, RSD 0.9-2.6, n=3 and 86-96%, RSD 3-8%, n=5, respectively). The novel sol-gel hybrid MTMOS-TEOS SPE sorbent demonstrate the potential as an alternative inexpensive extraction sorbent for OPPs with higher sensitivity for the OPPs.

Matched MeSH terms: Solid Phase Extraction/methods*
Determination of mitragynine in plasma with solid-phase extraction and rapid HPLC-UV analysis, and its application to a pharmacokinetic study in rat

Parthasarathy S, Ramanathan S, Ismail S, Adenan MI, Mansor SM, Murugaiyah V

Anal Bioanal Chem, 2010 Jul;397(5):2023-30.
PMID: 20454783 DOI: 10.1007/s00216-010-3707-7

A new solid phase extraction method for rapid high performance liquid chromatography-UV determination of mitragynine in plasma has been developed. Optimal separation was achieved with an isocratic mobile phase consisting of acetonitrile-ammonium acetate buffer, 50 mM at pH 5.0 (50:50, v/v). The method had limits of detection and quantification of 0.025 and 0.050 microg/mL, respectively. The method was accurate and precise for the quantitative analysis of mitragynine in human and rat plasma with within-day and between-day accuracies between 84.0 and 109.6%, and their precision values were between 1.7 and 16.8%. Additional advantages over known methods are related to the solid phase extraction technique for sample preparation which yields a clean chromatogram, a short total analysis time, requires a smaller amount of plasma samples and has good assay sensitivity for bioanalytical application. The method was successfully applied in pharmacokinetic and stability studies of mitragynine. In the present study, mitragynine was found to be fairly stable during storage and sample preparation. The present study showed for the first time the detailed pharmacokinetic profiles of mitragynine. Following intravenous administration, mitragynine demonstrated a biphasic elimination from plasma. Oral absorption of the drug was slow, prolonged and was incomplete, with a calculated absolute oral bioavailability value of 3.03%. The variations observed in previous pharmacokinetic studies after oral administration of mitragynine could be attributed to its poor bioavailability rather than to the differences in assay method, metabolic saturation or mitragynine dose.

Matched MeSH terms: Solid Phase Extraction/methods*

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