scholarly journals New UHPLC-QqQ-MS/MS Method for the Rapid and Sensitive Analysis of Ascorbic and Dehydroascorbic Acids in Plant Foods

Molecules ◽  
2019 ◽  
Vol 24 (8) ◽  
pp. 1632 ◽  
Author(s):  
Nieves Baenas ◽  
Francisco J. Salar ◽  
Raúl Domínguez-Perles ◽  
Cristina García-Viguera

A new method using ultra high-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UHPLC-QqQ-MS/MS) methodology was developed for the determination of ascorbic acid (AA) and dehydroascorbic acid (DHAA) contents in liquid and solid vegetable samples. The advantages of this method are speed, high sensitivity and practical application. In accordance with these advantages, the present method allows the simultaneous determination of AA and DHAA without previous reduction/derivatization of DHAA and without the use of internal standards in the samples. This is of high interest in routine analysis, providing a simpler sample preparation, as well as enhanced accuracy and robustness. Its validation included selectivity, sensitivity and linearity, precision and accuracy, matrix effect, and recovery. The results showed high selectivity and sensitivity, with calibration curves ranging from 10 to 500 ng mL−1 and from 50 to 500 ng mL−1 for AA and DHAA, respectively. Appropriate dilutions for each sample are necessary to avoid the matrix effect with accepted recoveries.

2020 ◽  
Vol 23 (10) ◽  
pp. 1010-1022
Author(s):  
Emrah Dural

Aim and scope: Due to the serious toxicological risks and their widespread use, quantitative determination of phthalates in cosmetic products have importance for public health. The aim of this study was to develop a validated simple, rapid and reliable high-performance liquid chromatography (HPLC) method for the determination of phthalates which are; dimethyl phthalate (DMP), diethyl phthalate (DEP), benzyl butyl phthalate (BBP), di-n-butyl phthalate (DBP), di(2- ethylhexyl) phthalate (DEHP), in cosmetic products and to investigate these phthalate (PHT) levels in 48 cosmetic products marketing in Sivas, Turkey. Materials and Methods: Separation was achieved by a reverse-phase ACE-5 C18 column (4.6 x 250 mm, 5.0 μm). As the mobile phase, 5 mM KH2PO4 and acetonitrile were used gradiently at 1.5 ml min-1. All PHT esters were detected at 230 nm and the run time was taking 21 minutes. Results: This method showed the high sensitivity value the limit of quantification (LOQ) values for which are below 0.64 μg mL-1 of all phthalates. Method linearity was ≥0.999 (r2). Accuracy and precision values of all phthalates were calculated between (-6.5) and 6.6 (RE%) and ≤6.2 (RSD%), respectively. Average recovery was between 94.8% and 99.6%. Forty-eight samples used for both babies and adults were successfully analyzed by the developed method. Results have shown that, DMP (340.7 μg mL-1 ±323.7), DEP (1852.1 μg mL-1 ± 2192.0), and DBP (691.3 μg mL-1 ± 1378.5) were used highly in nail polish, fragrance and cream products, respectively. Conclusion: Phthalate esters, which are mostly detected in the content of fragrance, cream and nail polish products and our research in general, are DEP (1852.1 μg mL-1 ± 2192.0), DBP (691.3 μg mL-1 ± 1378.5) and DMP (340.7 μg mL-1 ±323.7), respectively. Phthalates were found in the content of all 48 cosmetic products examined, and the most detected phthalates in general average were DEP (581.7 μg mL-1 + 1405.2) with a rate of 79.2%. The unexpectedly high phthalate content in the examined cosmetic products revealed a great risk of these products on human health. The developed method is a simple, sensitive, reliable and economical alternative for the determination of phthalates in the content of cosmetic products, it can be used to identify phthalate esters in different products after some modifications.


Molecules ◽  
2021 ◽  
Vol 26 (14) ◽  
pp. 4357
Author(s):  
Waritda Pookmanee ◽  
Siriwan Thongthip ◽  
Jeeranut Tankanitlert ◽  
Mathirut Mungthin ◽  
Chonlaphat Sukasem ◽  
...  

The method for the determination of primaquine (PQ) and 5,6-orthoquinone primaquine (5,6-PQ), the representative marker for PQ active metabolites, via CYP2D6 in human plasma and urine has been validated. All samples were extracted using acetonitrile for protein precipitation and analyzed using the ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) system. Chromatography separation was carried out using a Hypersil GOLDTM aQ C18 column (100 × 2.1 mm, particle size 1.9 μm) with a C18 guard column (4 × 3 mm) flowed with an isocratic mode of methanol, water, and acetonitrile in an optimal ratio at 0.4 mL/min. The retention times of 5,6-PQ and PQ in plasma and urine were 0.8 and 1.6 min, respectively. The method was validated according to the guideline. The linearity of the analytes was in the range of 25–1500 ng/mL. The matrix effect of PQ and 5,6-PQ ranged from 100% to 116% and from 87% to 104% for plasma, and from 87% to 89% and from 86% to 87% for urine, respectively. The recovery of PQ and 5,6-PQ ranged from 78% to 95% and form 80% to 98% for plasma, and from 102% to from 112% to 97% to 109% for urine, respectively. The accuracy and precision of PQ and 5,6-PQ in plasma and urine were within the acceptance criteria. The samples should be kept in the freezer (−80 °C) and analyzed within 7 days due to the metabolite stability. This validated UHPLC-MS/MS method was beneficial for a pharmacokinetic study in subjects receiving PQ.


2021 ◽  
Author(s):  
Naeime Salandari-Jolge ◽  
Ali A. Ensafi ◽  
Behzad Rezaei

Dipyridamole is a prescribed medication used to treat cardiovascular diseases, angina pectoris, imaging tests for heart patients, and myocardial infarction. Therefore, high selectivity and sensitivity, low cost, and high-performance speed...


2016 ◽  
Vol 8 (2) ◽  
pp. 333-341 ◽  
Author(s):  
Renu Pandey ◽  
Preeti Chandra ◽  
Brijesh Kumar ◽  
Bhupender Dutt ◽  
Kulwant Rai Sharma

Ocimum species have tremendous value in pharmaceutical, perfumery, food processing and cosmetic industries, also in traditional rituals and medicines.


2021 ◽  
Author(s):  
Feng Gao ◽  
Xiaolong Tu ◽  
Yongfang Yu ◽  
Yansha Gao ◽  
Jin Zou ◽  
...  

Abstract Herein, an efficient electrochemical sensing platform is proposed for selective and sensitive detection of nitrite on the basis of Cu@C@Zeolitic imidazolate framework-8 (Cu@C@ZIF-8) heterostructure. Core-shell Cu@C@ZIF-8 composite was synthesized by pyrolysis of Cu-metal-organic framework@ZIF-8 (Cu-MOF@ZIF-8) in Ar atmosphere on account of the difference of thermal stability between Cu-MOF and ZIF-8. For the sensing system of Cu@C@ZIF-8, ZIF-8 with proper pore size allows nitrite diffuse through the shell, while big molecules cannot, which ensures high selectivity of the sensor. On the other hand, Cu@C as electrocatalyst promotes the oxidation of nitrite, thereby resulting high sensitivity of the sensor. Accordingly, the Cu@C@ZIF-8 based sensor presents excellent performance for nitrite detection, which achieves a wide linear response range of 0.1 µM to 300.0 µM, and a low limit of detection (LOD) of 0.033 µM. In addition, the Cu@C@ZIF-8 sensor possesses excellent stability and reproducibility, and was employed to quantify nitrite in sausage samples with recoveries of 95.45-104.80%.


2019 ◽  
Vol 97 (2) ◽  
pp. 140-146
Author(s):  
Tian Gan ◽  
Zhikai Wang ◽  
Mengru Chen ◽  
Wanqiu Fu ◽  
Haibo Wang ◽  
...  

In this work, the Ag@Cu particles with yolk–shell nanostructure was prepared by facile solvothermal method, which was modified on glassy carbon electrode (GCE) to fabricate electrochemical sensor for the convenient and fast determination of p-aminobenzoic acid (PABA). The surface morphology and electrochemical properties of the as-prepared Ag@Cu nanocomposite modified electrode were characterized by scanning electron microscopy, transmission electron microscopy, chronocoulometry, and electrochemical impedance spectroscopy. Further, the electrochemical sensing of PABA was performed on the Ag@Cu/GCE using cyclic voltammetry and differential pulse voltammetry techniques, showing high catalytic activity. Under the optimal conditions, the sensor exhibited a wide linear range, high sensitivity, and low detection limit of 0.315 μmol/L for PABA. The developed sensor was also successfully applied for PABA detection in anesthetic and cosmetics with satisfactory results.


2000 ◽  
Vol 283-287 ◽  
pp. 1006-1010 ◽  
Author(s):  
B.M Oliver ◽  
F.A Garner ◽  
L.R Greenwood ◽  
J.A Abrefah

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