scholarly journals APPROACHES TO CHORIONIC GONADOTROPIN QUANTITATIVE DETERMINATION IN ANTI-DOPING CONTROL

2017 ◽  
Vol 12 (1) ◽  
pp. 64-75 ◽  
Author(s):  
I. O. Zvereva ◽  
N. B. Savelieva ◽  
P. V. Postnikov ◽  
Yu. A. Efimova ◽  
M. A. Dikunets
Keyword(s):  
Chorionic Gonadotropin ◽  
High Performance ◽  
Quantitative Method ◽  
High Accuracy ◽  
Core Fragment ◽  
Stage Of Development ◽  
Applied Optimization ◽  
Hybrid Mass Spectrometer ◽  
Positive Results

The article presents the results of the first stage of development of a new quantitative method for human chorionic gonadotropin (hCG) determination by means of ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) to uncover doping abuse by athletes. The identified tryptic peptides correspond to the most abundant hCG isoforms: the α- and β-subunits, the nicked and β-core fragment of the hormone. Identification and sequencing of specific fragments were performed with the use of nanoLC-MS/MS. A high resolution / high accuracy hybrid mass-spectrometer was applied. Optimization of mass-spectrometric determination of selected specific peptides was accomplished by UPLC-MS/MS. Quantitative evaluation of hCG using specific fragments determination by UPLC-MS/MS allows to detect corresponding hCG isoforms. This significantly increases the method specificity and decreases the probability of false-positive results.

scholarly journals False-Negative Results in Point-of-Care Qualitative Human Chorionic Gonadotropin (hCG) Devices Due to Excess hCGβ Core Fragment

2009 ◽  
Vol 55 (7) ◽  
pp. 1389-1394 ◽  
Author(s):  
Ann M Gronowski ◽  
Mark Cervinski ◽  
Ulf-Håkan Stenman ◽  
Alison Woodworth ◽  
Lori Ashby ◽  
...  
Keyword(s):  
Chorionic Gonadotropin ◽  
Human Chorionic Gonadotropin ◽  
Point Of Care ◽  
False Negative ◽  
The Core ◽  
Core Fragment ◽  
Negative Results ◽  
False Negative Results ◽  
Positive Results ◽  
Urine Specimens

Abstract Background: During pregnancy, human chorionic gonadotropin (hCG) immunoreactivity in urine consists of intact hCG as well as a number of hCG variants including the core fragment of hCGβ (hCGβcf). We identified 3 urine specimens with apparent false-negative results using the OSOM® hCG Combo Test (Genzyme Diagnostics) qualitative hCG device and sought to determine whether an excess of 1 of the fragments or variants might be the cause of the interference. Methods: We measured concentrations of hCG variants in the urine from 3 patients with apparent false-negative hCG results. Purified hCG variants were added to urines positive for hCG and tested using the OSOM, ICON® 25 hCG (Beckman Coulter), and hCG Combo SP® Brand (Cardinal Health) devices. Results: Dilution of these 3 urine samples resulted in positive results on the OSOM device. Quantification of hCG variants in each of the 3 patient urine specimens demonstrated that hCGβcf occurred in molar excess of intact hCG. Addition of purified hCGβcf to hCG-positive urines caused false-negative hCG results using the OSOM and ICON qualitative urine hCG devices. Conclusions: Increased concentrations of hCGβcf can cause false-negative results on the OSOM and ICON qualitative urine hCG devices. .

scholarly journals Development and Validation of a HPLC-UV Method with Pre-column Derivatization for Determination of Cinnabar in Jufang Zhibao Pills

2017 ◽  
Vol 5 (02) ◽  
pp. 01-09
Author(s):  
Xin Zhang ◽  
Jia Yao ◽  
Ying Ren ◽  
Yuan Li ◽  
Zhimin Xie
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
High Accuracy ◽  
Chromatography Method ◽  
Average Recovery ◽  
Sem Image ◽  
Good Repeatability ◽  
Liquid Chromatography Method ◽  
Development And Validation

In this work, a reliable and accurate high-performance liquid chromatography method with pre-column derivatization was established and validated for determination of cinnabar in Jufang Zhibao pills. Scanning electron microscope (SEM) image was used to identify the types of cinnabar crude drug in Jufang Zhibao pills. The chromatography separation was performed on a Welch XB-C18 column (250 mm × 4.6 mm, 5 μm). The mobile phase consists of water spiked with 0.022 mmol/L sodium diethyldithiocarbamate (A, pH adjusted to 8–9 by ammonia water) and methanol (B, 80:20, v/v) at flow rate of 1.0 ml/min with the detected wavelength was 272 nm. The oven temperature was set at 35°C. The calibration for cinnabar content has good linearity (R2 =0.9999) over the range of 2.43–300 μg/ml and the average recovery was less then 1.90%. The limits of detection and quantification were 0.1127 μg and 0.2065 μg/ml. The results indicated that the proposed method has advantages of high accuracy, good repeatability and stability and can be successfully used for determination of cinnabar in Jufang Zhibao pills. It provides a basis for drug manufacture quality control and proves the feasibility of the pre-column derivatization method during the determination of cinnabar in Jufang Zhibao pills.

scholarly journals PALLADIUM (II) CHLORIDE (PdCl2) SPECTROPHOTOMETRY TO DETERMINE LIPOIC ACID CONCENTRATION IN PLASMA AND LEUKOCYTES

2020 ◽  
Vol 3 (1) ◽  
pp. 14-22
Author(s):  
Novian Agni Yudhaswara ◽  
Ani Retno Prijanti ◽  
Mohamad Sadikin
Keyword(s):  
High Performance Liquid Chromatography ◽  
Lipoic Acid ◽  
Pyruvate Dehydrogenase ◽  
Body Fluid ◽  
High Performance ◽  
Chelating Agent ◽  
High Accuracy ◽  
Hplc Measurement ◽  
Acid Determination

Background: Lipoic acid is a substance contained in intra and extracellular that act as a coenzyme of Pyruvate Dehydrogenase, also as an antidote, chelating agent and antioxidant. Measurement of lipoic acid is needed to determine the amount of lipoic acid that performs its functions either as a coenzyme or an antioxidant. Besides, this measurement requires a special tool such as High Performance Liquid Chromatography (HPLC) and a process that is available in rural or simple laboratories.  Objective: A common and easy tool such as a spectrophotometer was conducted and could expected to be a tool of lipoic acid determination in body fluid such as plasma.Methods: Measurement of lipoic acid using spectrophotometry with UV methanol and visible PdCl2 has been tested and compared to HPLC measurement that was valid and reliable in drug measurement or pharmaceutical preparations.Results: Determination of lipoic acid in plasma and leukocytes using PdCl2 produced replicable, reliability and valid result, with high accuracy, precision and was not different from lipoic acid measurement using HPLC, p=0.99. While UV methanol was different compare to HPLC p =0.0001 or was not valid.Conclusion: The measurement of lipoic acid using PdCl2 visible method can be applied to determine the levels of lipoic acid (LA) and DHLA in plasma and equal to HPLC result.

scholarly journals Solubility of Luteolin and Other Polyphenolic Compounds in Water, Nonpolar, Polar Aprotic and Protic Solvents by Applying FTIR/HPLC

Processes ◽  
2021 ◽  
Vol 9 (11) ◽  
pp. 1952
Author(s):  
Saša Rajhard ◽  
Lucija Hladnik ◽  
Filipa A. Vicente ◽  
Stanko Srčič ◽  
Miha Grilc ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
High Performance ◽  
Quantitative Method ◽  
Polyphenolic Compounds ◽  
Ftir Analysis ◽  
Initial Screening ◽  
Beneficial Effects ◽  
Protic Solvents ◽  
Shed Light

In recent years, flavonoids have become a highly researched topic due to their health beneficial effects. Since flavonoids’ solubility plays a significant role in their use in pharmaceutical, food, biological, and chemical areas, the determination of suitable solvents is crucial. Fourier transform infrared (FTIR) analysis was used to characterize functional groups of several flavonoids and phenolic compounds, namely luteolin, hesperidin, quercetin, naringenin, gallic acid and tannic acid. Concentration dependence on transmittance was evaluated for these compounds in ethanol. Afterwards, luteolin was chosen as a model flavonoid, with its concentration correlated with transmittance using 15 solvents with different polarities. Luteolin solubility was further corroborated with high-performance liquid chromatography (HPLC). These results shed light on using FTIR as a semi-quantitative method for the initial screening of solvents and the solubility of different compounds while saving time and solvents. Hence, HPLC would only be needed as a final step for the most promising solvents.

scholarly journals Determination of Nicotine Extracted from Eggplant and Green Pepper by HPLC

2019 ◽  
Vol 16 (1) ◽  
pp. 0061 ◽  
Author(s):  
Zeinab Hashim Mohammed
Keyword(s):  
Relative Error ◽  
High Performance ◽  
Standard Addition ◽  
High Accuracy ◽  
Green Pepper ◽  
Standard Material ◽  
Nicotine Concentration ◽  
Relative Recovery ◽  
Recovery Percentage

Nicotine was separated from eggplant and green pepper seeds (Solanaceous) by High Performance Liquid Chromatography (HPLC).The concentration of nicotine in the eggplant extract (0.871-0.877 μg/ml) was determined by injecting standard material with 0.5 and 1.5 μg/ml, while the concentrations of nicotine in green pepper extract (0.613-0.618 μg/ml) was determined when the standard material was injected with 0.5 and 1.5 μg/ml. The qualitative chemical data was calculated from derivations of the standard material. Nicotine concentration was measured qualitatively in both extracts through the calibration curve and method of the standard addition. This technique has high accuracy and compatibility, bringing the proportion of relative recovery percentage of nicotine extracted from eggplant seeds to 95.880-103.104% and relative error of -4.119-3.104%. Relative recovery percentage   of nicotine extracted from green pepper seeds was 97.284 -103.518 % and relative error was -2.716-3.518%.

scholarly journals Comparison of enzyme linked immunoassay and high performance liquid chromatography for determination of fumonisin in dried figs

2009 ◽  
pp. 37-43 ◽  
Author(s):  
Funda Karbancioglu-Guler ◽  
Dilek Heperkan
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
False Positive ◽  
High Performance ◽  
Screening Method ◽  
Fumonisin B1 ◽  
Aegean Region ◽  
Positive Results

The occurrence of fumonisin in dried figs was investigated by Enzyme Linked Immunoassay (ELISA) and High Performance Liquid Chromatography (HPLC). Total fumonisins (FB1, FB2, FB3) in dried figs were determined using ELISA, whereas only fumonisin B1 (FB1) was determined by HPLC. In the period 2003-2004, one hundred and fifty five dried fig samples were taken during their drying in 7 different districts in the Aegean Region. Among a total of 115 samples, the incidence of total fumonisin in the dried figs was 82% within the range of 0.16 - 108.34 mg/g when determined by ELISA. In comparison, FB1 was detected in 86 samples (74.8%) within the range between 0.046 and 3.649 mg/g by HPLC. Correlation between ELISA and HPLC methods was observed for all samples. However, no correlation between methods was recorded for the samples with less than 1 mg/g Fumonisin B1 level (obtained by HPLC). Although there was a correlation between methods for all the samples, fumonisin levels obtained by ELISA were much higher than those obtained by HPLC. False positive results were obtained by ELISA in 11 out of 115 dried fig samples. The results indicated that ELISA can be used as a screening method for determining the occurence of fumonisin in dried figs.

scholarly journals Respiratory alkalosis does not alter NOx concentrations in human plasma and erythrocytes

2001 ◽  
Vol 281 (6) ◽  
pp. H2757-H2761 ◽  
Author(s):  
Takaharu Ishibashi ◽  
Kaname Kubota ◽  
Mariko Himeno ◽  
Taku Matsubara ◽  
Tomoyuki Hori ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Whole Blood ◽  
Blood Cells ◽  
High Performance ◽  
Respiratory Alkalosis ◽  
High Accuracy ◽  
Reverse Phase ◽  
Phase Column

To test the hypothesis that NOx (NO[Formula: see text] and NO[Formula: see text], metabolites of NO) accumulates in red blood cells (RBC) in response to changes in Pco 2 and bicarbonate (HCO[Formula: see text]) concentration in blood, we examined the effect of changes in Pco 2 and HCO[Formula: see text] induced by hyperventilation in healthy adults on partitioning of NOx in whole blood. NOx in hemolysate was measured by a high-performance liquid chromatography-Griess system equipped with a C18 reverse phase column to trap hemoglobin, which enables determination of whole blood NOx concentration and calculation of NOx concentration in RBC with high accuracy and reproducibility. NOx concentration in RBC was lower than that in plasma, and equilibrium between plasma and RBC was achieved rapidly after addition of NO[Formula: see text]. Changes in Pco 2 and HCO[Formula: see text] by hyperventilation failed to influence NOx concentrations in both plasma and RBC. Plasma NOx concentrations correlated with whole blood NOx and RBC NOx concentrations. Our results indicate that changes in Pco 2 or HCO[Formula: see text] induced by hyperventilation do not influence NOx compartmentalization in plasma and RBC.

scholarly journals The Determination of Benzo[a]Pyrene and Benz[a]Anthracene in Mainstream and Sidestream Smoke of the Kentucky Reference Cigarette 1R4F and a Cigarette Which Heats but Does Not Burn Tobacco: A Comparison

1991 ◽  
Vol 15 (1) ◽  
pp. 11-17 ◽  
Author(s):  
CH Risner
Keyword(s):  
High Performance Liquid Chromatography ◽  
Aromatic Hydrocarbons ◽  
High Performance ◽  
Quantitative Method ◽  
Normal Phase ◽  
Tobacco Company ◽  
Reverse Phase ◽  
Sidestream Smoke ◽  
Polycyclic Aromatic

AbstractA quantitative method for the determination of benz[a]anthracene (B[a]A) and benzo[a]pyrene (B[a]P) in mainstream and sidestream cigarette smoke by high performance liquid chromatography (HPLC) has been developed. Mainstream and sidestream particulate matter is collected on Cambridge filter pads. The polycyclic aromatic hydrocarbons (PAH) are extracted with cyclohexane and subjected to normal-phase chromatography to isolate target fractions which are concentrated and then diluted with acetonitrile or acetonitrile/water prior to reverse-phase analytical chromatography. The Kentucky Reference cigarette 1R4F and a cigarette which heats but does not burn tobacco (New Cigarette) developed at R.J. Reynolds Tobacco Company were analysed and compared with respect to B[a]P and B[a]A in both mainstream and sidestream smoke.

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