scholarly journals Optimizing methods to characterize caffeic, ferulic, and chlorogenic acids in Salicornia sinus-persica and Salicornia bigelovii extracts by tandem mass spectrometry (LC-MS/MS)

BioResources ◽  
2021 ◽  
Vol 16 (3) ◽  
pp. 5508-5523
Author(s):  
Iwona Cybulska ◽  
Joanna Zembrzuska ◽  
Grzegorz Brudecki ◽  
Mette Hedegaard Thomsen

Three types of phenolic acids (caffeic, ferulic, and chlorogenic acid) were identified and quantified in two halophytic plants (Salicornia bigelovii and Salicornia sinus-persica). Analysis was performed using a high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) system via the standard addition method. The matrix effect (ME), recovery efficiency (RE), and process efficiency (PE) parameters were evaluated for S. bigelovii extracts, which revealed a strong ME on the ionization of the three acids. The matrix had little to no effect on the extraction step for all samples. The quantitation results revealed that S. bigelovii was more abundant in the acids analyzed (total of 319.2 µg/g dry water extract) when compared to S. sinus-persica (117.2 µg/g dry water extract), and chlorogenic acid was the dominant component. The extractives content was high in both plants, representing over 35% of the dry plant weight. All the extracts exhibited antioxidant activity toward both DPPH and ABTS radicals at levels comparable to other medicinal plants.

2017 ◽  
Vol 40 (6) ◽  
pp. 1293-1300 ◽  
Author(s):  
Kazuhiko Akutsu ◽  
Masato Yoshimitsu ◽  
Yoko Kitagawa ◽  
Satoshi Takatori ◽  
Naoki Fukui ◽  
...  

Author(s):  
KR Allen ◽  
R Azad ◽  
HP Field ◽  
DK Blake

Background: There is increasing interest in the use of oral fluid as the matrix for the detection of drugs of abuse which requires the use of sensitive immunoassays to achieve the low detection limits required. The use of liquid chromatography linked to tandem mass spectrometry (LC/MS/MS) is explored as a possible replacement for immunoassay in screening for drugs of abuse in oral fluid samples. Methods: Oral fluid samples collected from 72 subjects attending an addiction clinic were screened for opiates, cocaine, methadone and benzodiazepines using both enzyme-linked immunosorbent assays (ELISA) and LC/MS/MS. The latter analysis used a short gradient elution with individual drugs detected by multiple reaction monitoring using tandem mass spectrometry. Results between the two methods were compared qualitatively using the cut-off concentrations defined by the ELISA assays. Results: With regard to the ELISA assays which show group specificity, LC/MS/ MS detected the presence of 6-monoacetylmorphine, morphine or dihydrocodeine in all but two of 49 samples positive for opiates. Of 55 samples positive for benzodiazepines by ELISA, all but two were confirmed by LC/MS/MS. Overall, LC/MS/MS compared favourably with ELISA for detection of specific drugs or their metabolites in the case of morphine, methadone and the cocaine metabolite benzoylecgonine. Many of the discrepant results between the two assays were a result of samples with drug concentrations near to the cut-off concentrations and the imprecision of these assays at very low concentrations. Conclusion: LC/MS/MS offers a more flexible, specific and sensitive alternative to the screening of oral fluid samples for drugs of abuse than ELISA. A wide range of drugs and metabolites can be detected from a single sample injection.


2021 ◽  
Author(s):  
MD Shachneva ◽  
MA Leninskii ◽  
EI Savelieva

Wipe sampling is widely used for microbiological control purposes. Sanitary and chemical studies also include analysis of samples wiped from the work surfaces during routine and periodic working conditions safety inspections at chemical facilities. The analysis also allows assessing the toxicity and hazard of items/structures that could be in contact with highly toxic substances. This study aimed to investigate the capabilities and limitations of the surface wipe sample analysis method in control of residual contamination of equipment and building structures of a former chemical weapons destruction facilities (CWDF) with sulfur mustard and O-isobutyl-S(2-diethylaminoethyl) methylphosphonothioate (VR), as well as their degradation products. Gas chromatography with tandem mass spectrometry (GC-MS/MS) enabled identification of the sulfur mustard markers, high-performance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS) allowed identifying VR markers. An assessment of the matrix influence on the results of GC-MS/MS and HPLC-MS/MS analysis was carried out. The matrix effect was established to affect the results the most in case of HPLC-MS/MS analysis: for GC-MS/MS analysis of target substances, the matrix factor averaged at 60–80%, for HPLC-MS/ MS it was less than 40%. The average percent sulfur mustard recoveries from three types of surfaces (PVC tiles, laminate and metal plates) was 9 ± 2%, 0.13 ± 0.02% and 0.10 ± 0.03%; in case of VR, the recoveries was 2.7 ± 0.5%, 11.8 ± 0.3% and 0.8 ± 0.1%, respectively. The limits of detection for sulfur mustard by GC-MS/MS and VR by HPLC-MS/MS were established at 0.001 MPL and 0.02 MPL, respectively. The developed approaches were applied to the analysis of wipe samples from the surfaces of the equipment and engineering structures of the former CWDF.


2012 ◽  
Vol 7 ◽  
pp. ACI.S9969 ◽  
Author(s):  
J.S. Li ◽  
M. Chen ◽  
Z.C. Li

A sensitive and reliable method of liquid chromatography–electrospray ionization/tandem mass spectrometry (LC-ESI/MS/MS) was developed and validated for determining 1,3-dimethylamylamine (1,3-DMAA) and 1,4-dimethylamylamine (1,4-DMAA) in geranium plants ( Pelargonium graveolens). The sample was extracted with 0.5 M HCl and purified by liquid-liquid partition with hexane. The parameters for reverse-phase (C18) LC and positive ESI/MS/MS were optimized. The matrix effect, specificity, linearity, precision, accuracy and reproducibility of the method were determined and evaluated. The method was linear over a range of 0.10-10.00 ng/mL examined, with R 2 of 0.99 for both 1,3-DMAA and 1,4-DMAA. The recoveries from spiked concentrations between 5.00-40.00 ng/g were 85.1%-104.9% for 1,3-DMAA, with relative standard deviation (RSD) of 2.9%-11.0%, and 82.9%-101.8% for 1,4-DMAA, with RSD of 3.2%–-11.7%. The instrument detection limit was 1-2 pg for both DMAAs. The quantification limit was estimated to be 1-2 ng/g for the plant sample. This method was successfully applied to the quantitative determination of 1,3- and 1,4-DMAA in both geranium plant and geranium oil.


2021 ◽  
Vol 2021 ◽  
pp. 1-7
Author(s):  
Chaonan Han ◽  
Xiuqin Li ◽  
Hui Jiao ◽  
Yan Gao ◽  
Qinghe Zhang

Liquid chromatography-tandem mass spectrometry (LC-MS/MS) is the most commonly used method for sulfonamide determination. Its accuracy, however, can be affected by many factors. In this study, sulfadiazine (SDZ), sulfadimidine (SMZ), and sulfadimethoxine (SDM) in milk were selected to investigate an accurate determination method and the potential influencing factors in the use of ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Milk samples were extracted by 25 mL perchloric acid solution (pH = 2) and cleaned up using HLB solid-phase extraction (SPE) cartridges. Four kinds of filters, including PTFE, GHP, nylon, and glass fiber, were compared, and PTFE was selected since it had the best recoveries of target sulfonamides (SAs). Three quantitative methods, including external standard (ES), matrix matching (MM), and isotope dilution mass spectrometry (IDMS), were compared, among which IDMS exhibited the best accuracy. The matrix effect under different mobile phase compositions and of different sample matrices were evaluated and discussed. Ion suppression effects were observed during the determination of all SAs, which got stronger with the increase of the methanol composition percent in the mobile phase. After correction by IDMS, the matrix effect could be neglected. Matrix spiked recoveries at three spiked levels (1 μg/kg, 10 μg/kg, and 20 μg/kg) ranged from 96.8% to 103.8% by IDMS. The expanded relative uncertainties were in the range of 2.02% to 5.75%. The method exhibited wide application range, high accuracy, good stability, and high sensitivity.


Sign in / Sign up

Export Citation Format

Share Document