scholarly journals Quantification of 17 Endogenous and Exogenous Steroidal Hormones in Equine and Bovine Blood for Doping Control with UHPLC-MS/MS

2021 ◽  
Vol 14 (5) ◽  
pp. 393
Author(s):  
Giovanni Caprioli ◽  
Michele Genangeli ◽  
Ahmed M. Mustafa ◽  
Riccardo Petrelli ◽  
Massimo Ricciutelli ◽  
...  

A simple and fast analytical method able to simultaneously identify and quantify 17 endogenous and exogenous steroidal hormones was developed in bovine and equine blood using UHPLC-MS/MS. A total amount of 500 µL of sample was deproteinized with 500 µL of a mixture of methanol and zinc sulfate and evaporated. The mixture was reconstituted with 50 µL of a solution of 25% methanol and injected in the UHPLC-MS/MS triple quadrupole. The correlation coefficients of the calibration curves of the analyzed compounds were in the range of 0.9932–0.9999, and the limits of detection and quantification were in the range of 0.023–1.833 and 0.069–5.5 ppb, respectively. The developed method showed a high sensitivity and qualitative aspects allowing the detection and quantification of all steroids in equine and bovine blood. Moreover, the detection limit of testosterone (50 ppt) is half of the threshold admitted in plasma (100 ppt). Once validated, the method was used to quantify 17 steroid hormones in both bovine and equine blood samples. The primary endogenous compounds detected were corticosterone (range 0.28–0.60 ppb) and cortisol (range 0.44–10.00 ppb), followed by androstenedione, testosterone and 11-deoxycortisol.

2014 ◽  
Vol 79 (12) ◽  
pp. 1537-1543 ◽  
Author(s):  
Vele Tesevic ◽  
Ivana Aljancic ◽  
Vlatka Vajs ◽  
Marijana Zivkovic ◽  
Ninoslav Nikicevic ◽  
...  

An ultra-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-QqQ-MS/MS) method with multiple reactions monitoring mode (MRM) has been developed and validated for quantification of vanillin and syringaldehyde in plum brandy. The method showed good linearity (0.05 to 10 mgL?1) and low limits of detection and quantification (LOD and LOQ were 11.6 ?gL?1 and 38.2 ?gL?1 for vanillin, and 12.7 ?gL?1 and 42.0 ?gL?1 for syringaldehyde, respectively). The overall intra-day and inter-day variations were less than 4.21%, and the overall recovery over 93.0%. The correlation coefficients (R2) of the calibration curves were higher than 0.9999. In order to evaluate if the method is suitable for use as a routine analytical tool, in 31 Serbian plum brandy samples vanillin and syringaldehide were determined.


Author(s):  
Jianbing Wu ◽  
Fang Zhang ◽  
Xing Ke ◽  
Wei Jia ◽  
xuzhi wan ◽  
...  

Synthetic cannabinoids are a series of synthetic substances that mimic the effects of natural cannabinoids and produce a much stronger toxicity than natural cannabinoids, which have become the most abused family of new psychoactive substances. A solid-phase extractive-liquid chromatography-triple quadrupole/linear ion trap mass spectrometry method was developed to determine 11 synthetic cannabinoids in rat urine. The factors affecting recovery were optimized, and Oasis HLB was selected to extract synthetic cannabinoids simultaneously. The results showed that the linear correlation coefficients of the synthetic cannabinoids ranged from 0.993 to 0.999, and the limit of quantitation ranged from 0.01 to 0.1 ng/mL, and the spiked recoveries ranged from 69.90% to 118.39%. This method has the advantages of good purification ability, simple operation, and good reproducibility, and can be used for the high sensitivity analysis of various synthetic cannabinoids in urine.


1993 ◽  
Vol 37 ◽  
pp. 599-605 ◽  
Author(s):  
T. Utaka ◽  
T. Shoji ◽  
K. Shimizu ◽  
T. Arai ◽  
R. Wilson

Total reflection X-ray Fluorescence (TXRF) has been applied to the detection and quantification of metal contamination on the surface and near-surface regions of silicon wafers in the semiconductor industry The need for improving the sensitivity and detection limit of the TXRF technique is driven by the progress in producing thinner films and finer features in the development of larger Mbit DRAMS.


2021 ◽  
pp. 2101511
Author(s):  
Ziwei Chen ◽  
Haojie Guo ◽  
Fusheng Zhang ◽  
Xiaowen Li ◽  
Jiabing Yu ◽  
...  

2021 ◽  
Vol 58 (3) ◽  
pp. 1-10
Author(s):  
Elena-Cornelia Mitran ◽  
Irina-Mariana Sandulache ◽  
Cristina-Mihaela Lite ◽  
Lucian Gabriel Radu

In time the environmental conditions could damage textiles (materials/ artifacts) causing the need to develop better non-destructive or at least micro-destructive analysis techniques of the samples. There are ethnographic textile artifacts that were treated in the past with various pesticides, that have not been mentioned in any document. These are often re-treated with chemicals by museum staff as a method of preventing pest infestation. Due to the progressive use of many pesticides, this paper was focused on the detection and quantification of three pesticides: malathion, methoxychlor, and permethrin (cis- and trans- isomers). Gas chromatography is one of the most widely used analytical techniques for characterizing volatile organic compounds and therefore was the analytical method of choice for the present study. Because these analytes are found at trace levels, the detection and quantification limits of analytes are very small and it is necessary to optimize and validate a SIM method - that allows the mass spectrometer to detect specific compounds with high sensitivity. In SIM mode, the instrument is set to collect data at selected masses of interest, thus increasing the accuracy and precision of the quantitative results. The present paper is aimed to develop this type of method with specificity and selectivity, high precision (expressed in terms of repeatability and intermediate accuracy), accuracy, suitable working range and linearity, and high degree of series� homogenity.


2013 ◽  
Vol 823 ◽  
pp. 291-295 ◽  
Author(s):  
Shou Chen Chai ◽  
Peng Yang ◽  
Cheng Jia Yang ◽  
Chun Li Cai ◽  
Na Yu

In the space restricted airtight environment that people lives in, detecting harmful gas by miniature gas chromatography is the practical requirement at present, however, PIDs performance is key factor that restrict the application of miniature gas chromatography, the redesign of the detectors gas route in this paper aiming at improve detectors stability observably, and schemed out miniature PID with high sensitivity, low detection limit and fast response. The result of the experiment shows that the detection limit is 0.04ppm, the sensitivity is 101mv/ppm,the stability is 0.04×10-6/24h,meeting the project requirement. Keywords: photoionization detector; ionization chamber; sensitivity; detection limit;


Chemosensors ◽  
2021 ◽  
Vol 9 (11) ◽  
pp. 327
Author(s):  
Panxue Wang ◽  
Yan Sun ◽  
Li Wang ◽  
Xiang Li ◽  
Miaomiao Liu ◽  
...  

Rapid and facile determination of pesticides is critically important in food and environmental monitoring. This study developed a self-assembled gold nanoparticle array based SERS method for highly specific and sensitive detection of acetamiprid, a neonicotinoid pesticide that used to be difficult in SERS analysis due to its low affinity with SERS substrates. SERS detection and quantification of acetamiprid was conducted with self-assembled gold nanoparticle arrays at the interface of chloroform and water as the enhancing substrate. Since targets dissolved in chloroform (organic phase) also have access to the hot-spots of Au NP array, the developed method exhibited good sensitivity and specificity for acetamiprid determination. Under the optimal conditions, SERS intensities at Raman shifts of 631 cm−1 and 1109 cm−1 displayed a good linear relationship with the logarithm concentration of acetamiprid in the range of 5.0 × 10−7 to 1.0 × 10−4 mol/L (0.11335 ppm to 22.67 ppm), with correlation coefficients of 0.97972 and 0.97552, respectively. The calculated LOD and LOQ of this method were 1.19 × 10−7 mol/L (0.265 ppb) and 2.63 × 10−7 mol/L (0.586 ppb), respectively, using SERS signal at 631 cm−1, and 2.95 × 10−7 mol/L (0.657 ppb) and 3.86 × 10−7 mol/L (0.860 ppb) using SERS signal at 1109 cm−1, respectively. Furthermore, the developed SERS method was successfully applied in determining acetamiprid on the surface of apple and spinach. This method offers an exciting opportunity for rapid detection of acetamiprid and other organic pesticides considering its advantages of simple preparation process, good specificity and sensitivity, and short detection time (within 1 h).


2020 ◽  
Vol 36 (3) ◽  
pp. 329-339
Author(s):  
Nguyen Giang ◽  
Nguyen Hien ◽  
Huynh Loan ◽  
Phan Phuc ◽  
Nguyen Dai ◽  
...  

Serum profile is generally considered as comprehensive data which directly reflected animal health and their potential resistance to environmental, nutritional and pathological stress. The present study aimed to provide physiological reference values for selected biochemical parameters in Noi chickens, a famous Vietnamese native breed, at 56 days old. The collected blood samples of 355 Noi birds (164 males and 191 females) were used to evaluate biochemical serum profile. Glucose, total protein, albumin, globulin, albumin/globulin ratio, triglycerides, cholesterol, creatinine, and uric acid in the serum were measured. The variation in these values arising from different sexes was also investigated. The results indicated that there were no differences (P>0.05) in the assessed indices between male and female Noi chickens. In overall for the whole group, these values were obtained as 250.86 mg/dL, 7.34 g/dL, 3.40 g/dL, 3.94 g/dL, 1.75, 148.54 mg/dL, 190.86 mg/dL, 0.44 mg/dL, and 1.44 mg/dL, respectively. The relationship among the biochemical parameters showed relatively low coefficients (r=0.79 in maximum). The females obtained higher correlation coefficients between levels of total protein and glucose (r=0.42) as well as between total protein and globulin (r=0.79), compared to the males. It was concluded that the male and female chickens performed similar values of serum indices. The contribution of this study might expand the knowledge on the biochemical profile and improved breeding strategies of Vietnamese indigenous Noi chickens.


2021 ◽  
Author(s):  
Somia Ahmed ◽  
Hadeer Mohamed ◽  
Abeer Al-Subaie ◽  
Ahoud Al-Ohali ◽  
Nesrine Mahmoud

Abstract Novel synthesized Chitosan-Copper oxide nanocomposite (Cs-CuO) was prepared using pomegranate peels extract as green precipitating agents to improve the biological activity of Cs-NP's which was synthesized through ionic gelation method. The characterization of biogenic nanoparticles Cs-NP's and Cs-CuO-NP's were investigated structurally, morphologically to determine the full descriptive features of those nanoparticles. Antimicrobial activity was tested for both Cs-NP's and Cs-CuO-NP's via Minimum inhibition concentration and zone analysis against fungus, gram positive and gram negative. The results of the antimicrobial test showed high sensitivity of Cs-CuO-NP's to all microorganisms that are tested in concentration less than 20 mg/ml while the sensitivity of Cs-NP's against all microorganisms under test started from a concentration of 20 mg/ml to 40 mg/ml except for the C.albicans species. Hematological activity was also tested in via measuring the RBCs, platelets count and clotting time against healthy, diabetic and hypercholesterolic blood samples. Measurement showed a decrease in RBCs and platelets count by adding Cs-NP’s or Cs-CuO-NP's to the three blood samples. Cs-NP’s success to decrease the clotting time for healthy and diabetic blood acting as a procoagulant agent, while adding biogenic CuO-NP’s to Cs-NP’s increased clotting time considering as an anticoagulant agent for hyperchloesterolic blood samples.


Molecules ◽  
2021 ◽  
Vol 26 (19) ◽  
pp. 5955
Author(s):  
Qi-Ying Weng ◽  
Ya-Li Zhao ◽  
Jia-Ming Li ◽  
Miao Ouyang

A pair of cobalt(II)-based hydrogen-bonded organic frameworks (HOFs), [Co(pca)2(bmimb)]n (1) and [Co2(pca)4(bimb)2] (2), where Hpca = p-chlorobenzoic acid, bmimb = 1,3-bis((2-methylimidazol-1-yl)methyl)benzene, and bimb = 1,4-bis(imidazol-1-ylmethyl)benzene were hydrothermally synthesized and characterized through infrared spectroscopy (IR), elemental and thermal analysis (EA), power X-ray diffraction (PXRD), and single-crystal X-ray diffraction (SCXRD) analyses. X-ray diffraction structural analysis revealed that 1 has a one-dimensional (1D) infinite chain network through the deprotonated pca− monodentate chelation and with a μ2-bmimb bridge Co(II) atom, and 2 is a binuclear Co(II) complex construction with a pair of symmetry-related pca− and bimb ligands. For both 1 and 2, each cobalt atom has four coordinated twisted tetrahedral configurations with a N2O2 donor set. Then, 1 and 2 are further extended into three-dimensional (3D) or two-dimensional (2D) hydrogen-bonded organic frameworks through C–H···Cl interactions. Topologically, HOFs 1 and 2 can be simplified as a 4-connected qtz topology with a Schläfli symbol {64·82} and a 4-connected sql topology with a Schläfli symbol {44·62}, respectively. The fluorescent sensing application of 1 was investigated; 1 exhibits high sensitivity recognition for Fe3+ (Ksv: 10970 M−1 and detection limit: 19 μM) and Cr2O72− (Ksv: 12960 M−1 and detection limit: 20 μM). This work provides a feasible detection platform of HOFs for highly sensitive discrimination of Fe3+ and Cr2O72− in aqueous media.


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