scholarly journals Determination of Organophosphorus Esters in Fall Protection Equipment by Accelerated Solvent Extraction and Solid-Phase Extraction Coupled with LC-MS/MS Detection

2021 ◽  
Vol 2021 ◽  
pp. 1-7
Author(s):  
Haihong Li ◽  
Mingli Ye ◽  
Fangfang Wu ◽  
Xuyang Zhao ◽  
Lifeng Wang ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Solvent Extraction ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Accelerated Solvent Extraction ◽  
Phase Extraction ◽  
Water Mixture ◽  
Potential Health ◽  
Relative Standard ◽  
Fall Protection

An analysis method was established to determine 14 organophosphorus ester (OPE) flame retardants in fall protection equipment by combining accelerated solvent extraction (ASE) and solid-phase extraction (SPE) with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The ASE parameters were optimized as follows: static extraction with acetonitrile at 80°C for 5 min for two cycles. The combined extract was purified with the ENVI-18 cartridge before further analysis. A HILIC column was used to separate the OPEs using an acetonitrile/water mixture as the mobile phase with the detection by the electrospray ionization mass spectrometry, which was operated under the positive mode. Under optimized conditions, the limit of detection for the target OPEs ranged in 0.015–1.33 ng/g, with a spike recovery of 71.6%–114% and a relative standard deviation of 0.8%–11.2%. The developed method was used to analyze OPEs in fall protection equipment (safety helmets and ropes), where OPEs were all detectable. Safety ropes displayed a higher concentration of OPEs than ones in safety helmets, with the pollutants being mainly triphenyl phosphate, 2-ethylhexyl diphenyl phosphate (EHDPP), tri(2-ethylhexyl) phosphate, and tri-n-butyl phosphate in the range of 11.07 ng/g‒815.53 ng/g. The EHDPP was the dominant compound in safety helmets with the concentration from 26.84 to 95.29 ng/g, while the other OPEs in safety helmets were lower than 5.136 ng/g. The potential health and environmental risks of these fall protection equipment during their use and disposal call for further attention.

scholarly journals Determination of Capsaicin and Dihydrocapsaicin in Some Chilli Varieties using Accelerated Solvent Extraction Associated with Solid-Phase Extraction Methods and RP-HPLC-Fluorescence

2012 ◽  
Vol 9 (3) ◽  
pp. 1550-1561 ◽  
Author(s):  
Saksit Chanthai ◽  
Jureerat Juangsamoot ◽  
Chalerm Ruangviriyachai ◽  
Suchila Techawongstien
Keyword(s):  
Solvent Extraction ◽  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Accelerated Solvent Extraction ◽  
Phase Extraction ◽  
Good Precision ◽  
Real Samples ◽  
Relative Standard

Reversed phase-HPLC with fluorescence detection of two major capsaicinoids was described. Isocratic elution using a ratio of methanol and deionized water (66:34, v/v) as mobile phase was used at a flow rate of 0.9 mL/min with well achieved separation within 6 min. Under optimum conditions, their analytical figures of merit for the HPLC method were validated. The linearity was in the range of 1.0-25.0 μg/mL with multiple determination coefficients of higher than 0.995. The limit of detection was ranged of 0.008-0.01 μg/mL. The repeatability and reproducibility of the retention time and peak area for these compounds were in good precision with their relative standard deviations (RSDs) lower than 1% and 5%, respectively. Both capsaicin and dihydrocapsaicin were extracted using an accelerated solvent extraction (ASE) of methanol as an extraction solvent for 5 min static time with 3 cycles. The methanolic extracts were subjected to clean up with C18solid-phase extraction (SPE) with its recoveries ranking of 90.2-98.0%. The method recoveries of real samples were found to be 60.7-98.6%. The optimized extraction method were applied for the determination of the two capsaicinoids in ten vareities of hot chilli pepper samples. Total contents of capsaicinoids were found in the range of 2,307.0-9047.3 μg/g DW with their corresponding Scoville heat unit (SHU) of 34,600-135,700. Additionally, the contents of capsaicinoids using external calibration method comparing with those of standard addition were not significantly different, indicating accuracy of the method. Mostly, the contents of capsaicin found in these real samples were rather higher than those of dihydrocapsaicin.

The Determination of Eight Pesticides in Panax notoginseng of Chinese Traditional Medicine Using Solid-Phase Extraction and Gas Chromatography-Mass Spectrometry

2012 ◽  
Vol 485 ◽  
pp. 68-71
Author(s):  
Na Wu ◽  
Yu Da Zhang ◽  
Wei Liu ◽  
Ping Yi ◽  
Ze Feng Wang ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Panax Notoginseng ◽  
Gas Chromatography Mass Spectrometry ◽  
Phase Extraction ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard

A simple and effective extraction method based on solid-phase extraction (SPE) was developed to determine chlorothalonil, metalaxyl, triadimefon, dimetachlone, procymidone, flumetralin, oxadixyl and iprodione in Panax Notoginseng using gas chromatography-mass spectrometry with selected ion monitoring (GC/MS, SIM). The prepared samples were analysed with GC-MS in the selected ion monitoring mode (SIM) using one target and two or three qualitative ions for each analyte. In the method, hexane - dichloromethane（6:4，v/v）was selected to effectively extract the pesticides from the Panax Notoginseng samples. Solid-phase extraction was carried out using Supelclean ENVI-Carb/NH2 SPE Column with acetonitrile-toluene (3:1, v/v) as the eluted solvent. In the linear range of each pesticide, the correlation coefficient was R2≥0.99. The limit of detection ranged from 0.001 to 0.05 µg.mL-1, average recoveries ranged from 79.80% to 95.00%, with relative standard deviations between 1.96% and 4.32% for all 8 pesticides.They were readily achieved with this method for all tested pesticides.

scholarly journals Simultaneous Determination of 23 Mycotoxins in Broiler Tissues by Solid Phase Extraction UHPLC-Q/Orbitrap High Resolution Mass Spectrometry

Separations ◽  
2021 ◽  
Vol 8 (12) ◽  
pp. 236
Author(s):  
Youyou Yang ◽  
Zhuolin He ◽  
Lei Mu ◽  
Yunfeng Xie ◽  
Liang Wang
Keyword(s):  
Mass Spectrometry ◽  
Solid Phase Extraction ◽  
Simultaneous Determination ◽  
Solid Phase ◽  
Harmful Effect ◽  
Phase Extraction ◽  
External Standard Method ◽  
Relative Standard ◽  
Limit Of Quantitation

Mycotoxins are a type of toxins harmful for not only animal but also human health. Cooccurrence of multi-mycotoxins could occur for food infected by several molds, producing multi-mycotoxins. It is necessary to develop corresponding determination methods, among which current mass spectrometry (MS) dominates. Currently, the accurate identification and quantitation of mycotoxins in complex matrices by MS with low resolution is still a challenge since false-positive results are typically obtained. Here, a method for the simultaneous determination of 23 mycotoxins in broiler tissues using ultra-high performance liquid chromatography-quadrupole/orbitrap HRMS was established. After the extraction by acetonitrile-water-formic acid (80:18:2, v/v/v), the purification by multifunctional purification solid phase extraction cartridges and the chromatographic separation on a C18 column, representative mycotoxins were determined by HRMS in full scan/data-dependent MS/MS acquisition mode. The quantitation was based on the external standard method. An MS/MS database of 23 mycotoxins was established to achieve qualitative screening and simultaneous quantification. Mycotoxins had a good linear relationship within a certain concentration range with correlation coefficients (r2) larger than 0.991 as well as the limit of quantitation of 1.80–300 μg/kg. The average recoveries at three different levels of low, medium and high fortification were 61–111% with relative standard deviations less than 13.5%. The method was fast, accurate, and suitable for the precise qualification of multiple mycotoxins in broiler tissues. 15 μg/kg zearalenone (ZEN) was detected in one liver sample among 30 samples from markets including chicken breast meat, liver, and gizzards. The result illustrated that the pollution of ZEN should not be neglected considering its harmful effect on the target organ of liver.

scholarly journals Determination of 24 Pesticides Residues in Leather Products by Solid-Phase Microextraction Coupled with Gas Chromatography–Mass Spectrometry

2020 ◽  
Vol 20 (4) ◽  
pp. 385-404
Author(s):  
Jinlan DAI ◽  
Honglei YIN ◽  
Hang WEI ◽  
Lei ZHOU ◽  
Minghua LIU
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Extraction Column ◽  
Phase Extraction ◽  
Mixed Solution ◽  
Pesticides Residues ◽  
Solid Phase Extraction Column ◽  
Relative Standard

Considering the high content of oil and complex residual additives in leather samples, a new analytical method based on the solid-phase extraction technique and gas chromatography-selected ion monitoring mass spectrometry (GC-SIM-MS) was developed to determine 24 organic compounds involving the organochlorine pesticides (OCPs), organophosphorous pesticides (OPPs) and pyrethroids pesticides residues in leather. The extraction conditions (such as the extraction solution, purification procedure and solid-phase extraction column) were optimized using the positive leather samples based on the recovery rates of the pesticides. The best extraction solution, solid-phase extraction column and chromatography column were n-hexane and ethyl acetate (1+1, volume) mixed solution, Carb-PSA (1.0 g, 6mL) and DB-1701 (length: 30 m, inside diameter: 0.25 mm, film thickness: 0.25 μm). The optimized extraction time and temperature were 20 min and 25°C, respectively. The detection limits of 24 pesticide residues range from 0.05 to 0.10 mg/kg, and the recoveries range from 74% to 116%. The relative standard deviations (RSD, n=6) range from 5.42% to 12.00%. The developed method presented a simple, rapid, sensitive, and inexpensive method to detect 24 pesticides in skin and leather and was successfully applied to the detect them in leather products (cowhide, sheep leather and pig leather).

scholarly journals Multiresidue Determination of Pesticides in Drinking and Related Waters by Gas Chromatography/Mass Spectrometry after Solid-Phase Extraction: Interlaboratory Study

2001 ◽  
Vol 84 (5) ◽  
pp. 1420-1430 ◽  
Author(s):  
François van Hoof ◽  
Peter van Wiele ◽  
Auguste Bruchet ◽  
Isabelle Schmitz ◽  
Ivana Bobeldiji ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Standard Deviation ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Tap Water ◽  
Bottled Water ◽  
Gas Chromatography Mass Spectrometry ◽  
Phase Extraction ◽  
Relative Standard

Abstract As part of a project funded by the European Commission (EC) for the development and evaluation of multiresidue methods for analysis of drinking and related waters, 15 European laboratories evaluated a method using styrene–divinylbenzene copolymer solid-phase extraction followed by gas chromatography/mass spectrometry. The main aim of the study was to evaluate whether the method meets the requirements of EC Directive 98/83 in terms of accuracy, precision, and detection limit for 22 pesticides according to the following requirements: limit of detection, ≤0.025 μg/L; accuracy, expressed as recovery between 75 and 125%; and precision, expressed as repeatability relative standard deviation of the method of <12.5% and as reproducibility relative standard deviation of the method of <25%. Analyses for unknown concentrations were performed with fortified commercial bottled and tap waters. All laboratories were able to achieve detection limits of 0.01 μg/L for all pesticides except dimethoate and desisopropylatrazine (0.02 μg/L). The criteria for repeatability were met for all compounds except trifluralin, dimethoate, and lindane in bottled water and chlorpyrifos, dimethoate, and lindane in tap water. The criteria for reproducibility were met for all compounds except trifluralin, dimethoate, and lindane in bottled water and pendimethalin, chlorpyrifos, dimethoate, terbutryn, and lindane in tap water. In terms of accuracy, the method meets the requirements for all pesticides in both matrixes, except for lindane in bottled water and lindane and chlorpyrifos in tap water.

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