A Dilute-and-Shoot Based UPLC-MS/MS Method for Multimycotoxins Analysis in Astragali radix

2019 ◽  
Vol 102 (4) ◽  
pp. 1186-1193 ◽  
Author(s):  
Yang-Fan Li ◽  
Yi Du ◽  
Jing-jie Zhao ◽  
Li Li ◽  
Hai Lin
Keyword(s):  
Cost Effective ◽  
Shanxi Province ◽  
Astragali Radix ◽  
Matrix Interferences ◽  
Extraction Solvent ◽  
Sample Extraction ◽  
Two Samples ◽  
Sensitive Determination ◽  
Good Determination

Abstract Background: Astragali radix is prone to be contaminated by various mycotoxins, leading to unpredictable threats on the quality and safety of Astragali radix and the health of the consumers. Therefore, the determination of multimycotoxins is imperative. Objective: To develop an efficient, sensitive, fast, and multianalyte method for detecting multimycotoxins in Astragali radix. Methods: A selective dilute-and-shoot pretreatment procedure based ultra-performance LC–tandem MS (UPLC-MS/MS) method was developed for sensitive determination of multimycotoxins in Astragali radix, including aflatoxin (AF) B1, B2, G1, G2, and ochratoxin A. The five mycotoxins were extracted by the dilute-and-shoot pretreatment procedure followed by UPLC-MS/MS detection. Types of sample extraction solvent, mobile-phase compositions and MS/MS parameters, and dilute-and-shoot conditions were optimized. Results: The optimized chromatographic and mass spectrometric conditions allowed the separation and detection of the five mycotoxins within 5 min. The validated UPLC-MS/MS method exhibited good sensitivity with LOD and LOQ lower than 0.2 and 0.5 μg/kg, respectively. RSD values for method precision were lower than 9%. Recoveries obtained were between 90.87 and 108.44% for all the analytes with RSDs of 3.96–8.03%. The developed method was applied for the detection of the 5 mycotoxins in 18 batches of Astragali radix with good determination performance and no matrix interferences. Two samples collected from Shanxi province and Neimenggu Autonomous Region in China were positive for AFB1 at 3.24 and 2.69 μg/kg, respectively. Conclusions: The dilute-and-shoot procedure allowed for the extraction of the mycotoxins with advantages of simple pretreatment, small extraction time, high selectivity and accuracy, as well as being cost effective and easy to operate without any clean-up steps. Highlights: This is the first report on dilute-and-shoot approach for mycotoxins extraction and detection in Chinese medicinal material matrixes.

Mass Spectrometry-Based Determination of Thyroid Hormones and Their Metabolites in Endocrine Diagnostics and Biomedical Research – Implications for Human Serum Diagnostics

2020 ◽  
Vol 128 (06/07) ◽  
pp. 358-374 ◽  
Author(s):  
Josef Köhrle ◽  
Keith H. Richards
Keyword(s):  
Wide Spectrum ◽  
Quantitative Detection ◽  
Matrix Interferences ◽  
Novel Technology ◽  
Sample Extraction ◽  
Recent Developments ◽  
Serum Diagnostics ◽  
Novel Applications ◽  
Total Concentrations

AbstractThe wide spectrum of novel applications for the LC-MS/MS-based analysis of thyroid hormone metabolites (THM) in blood samples and other biological specimen highlights the perspectives of this novel technology. However, thorough development of pre-analytical sample workup and careful validation of both pre-analytics and LC-MS/MS analytics, is needed, to allow for quantitative detection of the thyronome, which spans a broad concentration range in these biological samples.This minireview summarizes recent developments in advancing LC-MS/MS-based analytics and measurement of total concentrations of THM in blood specimen of humans, methods in part further refined in the context of previous achievements analyzing samples derived from cell-culture or tissues. Challenges and solutions to tackle efficient pre-analytic sample extraction and elimination of matrix interferences are compared. Options for automatization of pre-analytic sample-preparation and comprehensive coverage of the wide thyronome concentration range are presented. Conventional immunoassay versus LC-MS/MS-based determination of total and free THM concentrations are briefly compared.

Simultaneous separation and sensitive detection of four β2-agonists in biological specimens by CE-UV using a field-enhanced sample injection method

2015 ◽  
Vol 7 (1) ◽  
pp. 175-180 ◽  
Author(s):  
Cheng Chen ◽  
Lingchen Meng ◽  
Meixian Li ◽  
Zhiwei Zhu
Keyword(s):  
Cost Effective ◽  
Sensitive Detection ◽  
Injection Method ◽  
Sample Injection ◽  
Simultaneous Separation ◽  
Sensitive Determination ◽  
Β2 Agonists

A rapid, sensitive and cost-effective CE-UV method has been developed for the simultaneous separation and sensitive determination of four beta2-agonists.

scholarly journals Determination of carcinogenic herbicides in milk samples using green non-ionic silicone surfactant of cloud point extraction and spectrophotometry

2018 ◽  
Vol 5 (4) ◽  
pp. 171500 ◽  
Author(s):  
N. I. Mohd ◽  
N. N. M. Zain ◽  
M. Raoov ◽  
S. Mohamad
Keyword(s):  
Cloud Point ◽  
Cloud Point Extraction ◽  
Limit Of Detection ◽  
Cost Effective ◽  
Silicone Surfactant ◽  
Extraction Solvent ◽  
Milk Samples ◽  
Relative Standard ◽  
Limit Of Quantitation

A new cloud point methodology was successfully used for the extraction of carcinogenic pesticides in milk samples as a prior step to their determination by spectrophotometry. In this work, non-ionic silicone surfactant, also known as 3-(3-hydroxypropyl-heptatrimethylxyloxane), was chosen as a green extraction solvent because of its structure and properties. The effect of different parameters, such as the type of surfactant, concentration and volume of surfactant, pH, salt, temperature, incubation time and water content on the cloud point extraction of carcinogenic pesticides such as atrazine and propazine, was studied in detail and a set of optimum conditions was established. A good correlation coefficient ( R 2 ) in the range of 0.991–0.997 for all calibration curves was obtained. The limit of detection was 1.06 µg l −1 (atrazine) and 1.22 µg l −1 (propazine), and the limit of quantitation was 3.54 µg l −1 (atrazine) and 4.07 µg l −1 (propazine). Satisfactory recoveries in the range of 81–108% were determined in milk samples at 5 and 1000 µg l −1 , respectively, with low relative standard deviation, n  = 3 of 0.301–7.45% in milk matrices. The proposed method is very convenient, rapid, cost-effective and environmentally friendly for food analysis.

Sensitive determination of psychotropic drugs in urine samples using continuous liquid-phase microextraction with an extraction solvent lighter than water

2018 ◽  
Vol 42 (6) ◽  
pp. 4450-4456 ◽  
Author(s):  
Lida Haghnazari ◽  
Hamid Nomani ◽  
Nazir Fattahi ◽  
Kiomars Sharafi ◽  
Masoud Moradi
Keyword(s):  
Liquid Phase ◽  
Psychotropic Drugs ◽  
Urine Samples ◽  
Liquid Phase Microextraction ◽  
Extraction Solvent ◽  
Sensitive Determination ◽  
First Time

A novel extraction vessel was employed, for the first time, in continuous liquid-phase microextraction (CLPME) with an extraction solvent lighter than water for the extraction of psychotropic drugs from urine samples.

A Squaraine Derivative for Cost-Effective, Quick, and Highly Sensitive Determination of Mercury and Thiols and pH Sensing

ChemPlusChem ◽  
2016 ◽  
Vol 81 (9) ◽  
pp. 913-916 ◽  
Author(s):  
Alexandros A. Sklavounos ◽  
Eleftherios K. Pefkianakis ◽  
Dimitra K. Toubanaki ◽  
Georgios C. Vougioukalakis ◽  
Antony C. Calokerinos
Keyword(s):  
Cost Effective ◽  
Ph Sensing ◽  
Highly Sensitive ◽  
Sensitive Determination

scholarly journals Facile Preparation of Fe3O4/C Nanocomposite and Its Application for Cost-Effective and Sensitive Detection of Tryptophan

Biomolecules ◽  
2019 ◽  
Vol 9 (6) ◽  
pp. 245 ◽  
Author(s):  
Jun Liu ◽  
Shuai Dong ◽  
Quanguo He ◽  
Suchun Yang ◽  
Mei Xie ◽  
...  
Keyword(s):  
Human Serum ◽  
Cost Effective ◽  
X Ray Diffraction ◽  
Modified Glassy Carbon Electrode ◽  
Serum Samples ◽  
One Pot ◽  
Human Serum Samples ◽  
Sensitive Determination ◽  
The Cost

In this study, we reported facile synthesis of Fe3O4/C composite and its application for the cost-effective and sensitive determination of tryptophan (Trp) in human serum samples. Fe3O4/C composites were prepared by a simple one-pot hydrothermal method followed by a mild calcination procedure, using FeCl3∙6H2O as Fe3O4 precursor, and glucose as reducing agent and carbon source simultaneously. The Fe3O4/C composite modified glassy carbon electrode (Fe3O4/C/GCE) was prepared by drop-casting method. The microstructure and morphology of Fe3O4/C composite was characterized by powder X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. Due to large specific surface area and synergistic effect from Fe3O4 nanoparticles and carbon coating, Fe3O4/C composite showed excellent electrocatalytic activity toward the oxidation of Trp. As a result, the proposed Fe3O4/C/GCE displayed superior analytical performances toward Trp determination, with two wide detection ranges (1.0–80 μM and 80–800 μM) and a low detection limit (0.26 μM, S/N = 3). Moreover, successful detection of Trp in human serum samples further validate the practicability of the proposed sensor.

scholarly journals High-Frequency Heating Extraction Method for Sensitive Drug Analysis in Human Nails

Molecules ◽  
2018 ◽  
Vol 23 (12) ◽  
pp. 3231 ◽  
Author(s):  
Fumiki Takahashi ◽  
Masaru Kobayashi ◽  
Atsushi Kobayashi ◽  
Kanya Kobayashi ◽  
Hideki Asamura
Keyword(s):  
High Frequency ◽  
Extraction Method ◽  
Glass Tube ◽  
Drug Analysis ◽  
Test Tube ◽  
Extraction Solvent ◽  
Sensitive Determination ◽  
Human Nails ◽  
Frequency Heating

Background: A simple, sensitive, and rapid extraction method based on high-frequency (H-F) heating was developed for drug analysis in human nails. Methods: A human nail was placed in a glass tube with an extraction solvent (methanol and 0.1% formic acid; 7:3, v/v), and a ferromagnetic alloy (pyrofoil) was wrapped in a spiral around the glass tube. Then, the glass tube was placed in a Curie point pyrolyzer, and a H-F alternating voltage (600 kHz) was applied. The sample and extraction solvent were heated at the Curie temperature for 3 min. Different Curie temperatures were applied by changing the pyrofoil (160 °C, 170 °C, 220 °C, and 255 °C). Results: The caffeine in the nail was effectively and rapidly extracted into the extraction solvent with the pyrofoil at 220 °C. The peak area obtained for the caffeine using liquid chromatography mass spectrometry (LC-MS/MS) was five times that of what was obtained after conventional ultrasonic irradiation extraction. Because the extraction uses high-pressure and high-temperature conditions in a test tube, the drugs that were strongly incorporated in nails could be extracted into the solvent. The amount of caffeine extracted was independent of the size of the pieces in the sample. Conclusions: Therefore, the sensitive determination of target drugs in nails is possible with rapid (20 min, including H-F extraction for 3 min) and simple sample preparation. The developed method was applied to a nail from a patient with hypertension.

scholarly journals β-Cyclodextrin Assisted Liquid–Liquid Microextraction Based on Solidification of the Floating Organic Droplets Method for Determination of Neonicotinoid Residues

Molecules ◽  
2019 ◽  
Vol 24 (21) ◽  
pp. 3954
Author(s):  
Vichapong ◽  
Moyakao ◽  
Kachangoon ◽  
Burakham ◽  
Santaladchaiyakit ◽  
...  
Keyword(s):  
Pesticide Residues ◽  
Limit Of Detection ◽  
Environment Friendly ◽  
Extraction Solvent ◽  
Salt Addition ◽  
High Enrichment ◽  
Sensitive Determination ◽  
Cloudy Solution ◽  
Liquid Microextraction

An efficient and environment-friendly microextraction method, namely, β-cyclodextrin assisted liquid–liquid microextraction, based on solidification of the floating organic droplets method coupled with HPLC is investigated for the sensitive determination of trace neonicotinoid pesticide residues. In this method, β-cyclodextrin is used as a disperser solvent, while 1-octanol is selected as an extraction solvent. β-cyclodextrins was found to decrease interfacial tension and increase the contact area between the organic and water phases with the help of centrifugation. A cloudy solution was rapidly formed and then centrifuged to complete phase separation. Various key parameters influencing extraction efficiency were systematically investigated and optimized; they include salt addition, concentration of β-cyclodextrin, and volume of extraction solvent (1-octanol). Under optimum conditions, good linearity was obtained with coefficient for determination (R2) greater than 0.99. A low limit of detection, high enrichment factor, and good recovery (83 – 132) were achieved. This proves that the proposed method can be applied to determine trace neonicotinoid pesticide residues in natural surface water samples.

scholarly journals New Tb3+–simvastatin optical biosensor for sensitive determination of folic acid, progesterone, testosterone and vitamin D3 in biological fluids

RSC Advances ◽  
2021 ◽  
Vol 11 (52) ◽  
pp. 32861-32872
Author(s):  
Mohamed S. Attia ◽  
Amal M. Ahmed ◽  
Tarek A. Amin ◽  
Ahmed. O. Youssef ◽  
Mohammed A. Amin ◽  
...  
Keyword(s):  
Folic Acid ◽  
Vitamin D3 ◽  
Biological Fluids ◽  
Cost Effective ◽  
Optical Biosensor ◽  
Biological Compounds ◽  
Sensitive Determination ◽  
Photo Probe

An innovative, simple and cost effective Tb3+–simvastatin photo probe was designed and used as a core for a spectrofluorometric approach to sensitively determine four vital biological compounds in different matrices.

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