scholarly journals Determination of Pharmaceutical Residues by UPLC-MS/MS Method: Validation and Application on Surface Water and Hospital Wastewater

2021 ◽  
Vol 2021 ◽  
pp. 1-12
Author(s):  
Bui Van Hoi ◽  
Cam-Tu Vu ◽  
Lan-Anh Phung-Thi ◽  
Thao Thi Nguyen ◽  
Phuong Thanh Nguyen ◽  
...  
Keyword(s):  
Surface Water ◽  
Analytical Method ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Hospital Wastewater ◽  
Esi Ms ◽  
Pharmaceutical Residues ◽  
Detection Frequency

In this study, an analytical method for the simultaneous determination of 7 major pharmaceutical residues in Vietnam, namely, carbamazepine, ciprofloxacin, ofloxacin, ketoprofen, paracetamol, sulfamethoxazole, and trimethoprim, in surface water and hospital wastewater has been developed. The method includes enrichment and clean-up steps by solid phase extraction using mix-mode cation exchange, followed by identification and quantification using an ultrahigh-performance liquid chromatography and tandem mass spectrometry and employing electrospray ionization (UPLC-ESI-MS/MS). Seven target compounds were separated on the reversed phase column and detected in multiple reaction monitoring (MRM) mode within 6 minutes. The present study also optimized the operating parameters of the mass spectrometer to achieve the highest analytical signals for all target compounds. All characteristic parameters of the analytical method were investigated, including linearity range, limit of detection, limit of quantification, precision, and accuracy. The important parameter in UPLC-ESI-MS/MS, matrix effect, was assessed and implemented via preextraction and postextraction spiking experiments. The overall recoveries of all target compounds were in the ranges from 55% to 109% and 56 % to 115% for surface water and hospital wastewater, respectively. Detection limits for surface water and hospital wastewater were 0.005–0.015 µg L−1 and 0.014–0.123 µg L−1, respectively. The sensitivity of the developed method was allowed for determination of target compounds at trace level in environmental water samples. The in-house validation of the developed method was performed by spiking experiment in both the surface water and hospital wastewater matrix. The method was then applied to analyze several surface water and hospital wastewater samples taken from West Lake and some hospitals in Vietnam, where the level of these pharmaceutical product residues was still missed. Sulfamethoxazole was present at a high detection frequency in both surface water (33% of analyzed samples) and hospital wastewater (81% of analyzed samples) samples.

scholarly journals An LLE Based LC- ESI MS/MS Analytical Method Development to Detect Azithromycin Residue in Water to Monitor Contamination Level of River and Fish Farm of Bangladesh

2021 ◽  
Author(s):  
Md Humayun Kabir ◽  
Sabina Yasmin ◽  
Salma Akter Mou ◽  
Bushra Parvin Upoma ◽  
Shamim Ahmed ◽  
...  
Keyword(s):  
Analytical Method ◽  
Method Development ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Fish Farm ◽  
Contamination Level ◽  
Limit Of Quantification ◽  
Chromatographic Separations ◽  
Esi Ms ◽  
Multiple Reaction Monitoring Mode

Abstract The aim of this study to development and validate an analytical method to determine the Azithromycin (AZN) residue in water approach to monitor the contamination level of river and fish farm water of Bangladesh. Azithromycin (AZN) was analyzed using liquid chromatography mass spectrometry (LC-ESI MS/MS). The chromatographic separations of analyte were performed using ZORBAX RRHD Eclipse Plus C18 (2.1×100 mm, particle size 1.8 µm) column and mobile phase was 0.1% formic acid in water and acetonitrile with 50:50. The analyte were detected in positive electron spray ionization mode with multiple reaction monitoring mode (MRM) with mass transition from 749.5 m/z to 591 m/z and 158 m/z as quantifier and qualifier ion respectively. Liquid-liquid extraction method was used for the extraction of AZN residues. The developed method was validated in terms of accuracy, precision, linearity and specificity. The analyte showed a good linear in the range of 0.1-100 µg/L. Three spiking levels (0.25, 0.5 and 1.25 µg/L) was performed for determining accuracy and precision. Recoveries and RSD were in the range of 96.6-101.5% and 3.5-6.3 respectively. The estimated limit of detection and limit of quantification was 0.017 and 0.05 µg/L respectively. Using the developed method, we analyzed 5 different rivers and 5 different fish farm samples. We found no azithromycin residue in rivers water, but we found in one fish farm water azithromycin residue 0.35±0.06 µg/L. The results indicate that we should be concern to use antibiotics in fish farm water in different ways.

scholarly journals Simultaneous Determination of Methamphetamine and Its Isomer N-Isopropylbenzylamine in Forensic Samples by Using a Modified LC-ESI-MS/MS Method

2021 ◽  
Vol 2021 ◽  
pp. 1-9
Author(s):  
Yangxu Luo ◽  
Juan Du ◽  
Huadi Xiao ◽  
Ling Zheng ◽  
Xuncai Chen ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Acetate Solution ◽  
Accurate Identification ◽  
Esi Ms ◽  
Target Analytes ◽  
Relative Standard ◽  
Forensic Samples

Accurate identification and quantification of methamphetamine (MA) and its related substances are essential for the investigation and fair trial of drug offenses. In this study, a modified LC-ESI-MS/MS method for the simultaneous determination of MA and its isomer N-isopropylbenzylamine (N-IBA) in forensic samples was developed and validated. Optimum chromatographic separation of the target analytes was achieved on an Agilent Poroshell 120 SB-C18 column ( 4.6 × 100  mm, 2.7 μm) at 40°C with isocratic elution at the flow rate of 0.40 mL/min. The mobile phase was acetonitrile and 20 mM ammonium acetate solution containing 0.1% formic acid (80 : 20, v / v ). Positive ESI-MS/MS detection was performed in multiple reaction monitoring (MRM) mode to identify and quantify the target analytes. Method validation showed excellent linearity in the range of 0.51 ng/mL~51 ng/mL for MA and N-IBA. The low limit of detection (LLOD) and low limit of quantification (LLOQ) reached 0.1 ng/mL and 0.3 ng/mL for both analytes. The method showed a satisfactory accuracy with an inter- and intraday-relative error (RE) <20%, and a precision of inter- and intraday relative standard deviation (RSD) less than 15%. The validated method was successfully applied in real forensic samples and resulted in the detection of MA and N-IBA in 8 suspected samples in drug cases that only deemed MA positive using our previous routine screening procedure, which avoided the misidentification of N-IBA as MA.

Simultaneous Determination of Anionic, Amphoteric and Cationic Surfactants Mixtures in Surface Water

2018 ◽  
Vol 69 (1) ◽  
pp. 27-30 ◽  
Author(s):  
Iuliana Paun ◽  
Vasile Ion Iancu ◽  
Liliana Cruceru ◽  
Marcela Niculescu ◽  
Florentina Laura Chiriac
Keyword(s):  
Surface Water ◽  
Simultaneous Determination ◽  
Cationic Surfactants ◽  
Anionic Surfactants ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Acetate Solution ◽  
Limit Of Quantitation ◽  
Amphoteric Surfactants

A simple, reliable and accurate HPLC/CAD method was developed for the determination of anionic (sodium dioctyl sulfosuccinate and sodium 1-dodecane sulfonate), amphoteric (CHAPS (3-[(3-Cholamidopropyl) dimethylammonium]-1-propanesulfonate hydrate)) and cationic (benzethonium chloride) surfactants mixture from surface water samples. The chromatographic analysis was performed on an Acclaim Surfactant Plus (150 x 3.0 mm, 3 mm d.p.) column acquired from Thermo Scientific, kept at 300C. All experiments were performed in gradient elution conditions at a flow-rate of 0.6 mL/min. Mobile phase composition was a mixture of acetonitrile (A) and 0.1 M ammonium acetate solution acidified to pH 5 with acetic acid (B). The limit of detection (LD) were 20 mg/L for anionic surfactants and 30 mg/L for cationic and amphoteric surfactants. The calibration curves were linear between 15 mg/L � 110 mg/L, with R2 values above 0.992 for all surfactants. Solid phase extraction (SPE) using polymeric (Strata X) cartridges has been applied to extract and concentrate the target analytes from the synthetic samples. Surfactants recoveries after SPE procedure were situated between 91.5�94.6%. Intra-day and inter-day precision (RSD%) were situated between 4.0 � 7.7% and 7.5 � 11.7%, respectively. Limit of quantitation (LQ) was lower than 80 mg/L for anionic surfactants and 90 mg/L for cationic and 100 mg/L for amphoteric surfactants. The new sensitive and selective HPLC/CAD developed method allows simultaneous determination of anionic, amphoteric and cationic surfactants mixture from environmental samples (surface water).

Development of an analytical method for the simultaneous determination of the 17 EU Watch List compounds in surface waters: a Spanish case study

2018 ◽  
Vol 15 (8) ◽  
pp. 493
Author(s):  
José Luis Malvar ◽  
Concepción Abril ◽  
Julia Martín ◽  
Juan Luis Santos ◽  
Irene Aparicio ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Organic Pollutants ◽  
Surface Waters ◽  
Analytical Method ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Anthropogenic Activities ◽  
Watch List ◽  
The Eu

Environmental contextIn 2015, the European Union issued a Watch List of organic pollutants resulting from anthropogenic activities. A major obstacle to controlling these pollutants in the environment is the difficulty of their simultaneous measurement at low concentrations. We developed an analytical method for the simultaneous determination in surface water of the 17 pollutants included in the EU Watch List. AbstractA multi-class method was developed for the simultaneous determination of the 17 organic pollutants included in the EU Decision 2015/495 regarding surface waters. The target analytes were three estrogens, four pharmaceuticals, a food additive, a solar filter and eight pesticides. The target compounds were extracted through solid-phase extraction with Oasis HLB cartridges. Determination was carried out by high performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS). All compounds were satisfactorily determined in one single injection, with a chromatographic run time of only 20min. The limit of detection (LOD) of the proposed method was in the range of 0.08–13ngL−1. For most of the target compounds, except for 17α-ethinylestradiol, 17β-estradiol and estrone, the LOD values were equal or below those required by the EU Decision 2015/495. Accuracy was in the range of 69–120%, whereas inter-day variability was below 20% in all cases. The validated method was applied to assess the presence of these compounds in Mediterranean surface waters. Samples were collected from 18 sampling sites located in the south of Spain. Up to 14 compounds were detected, among them, the pharmaceutical compounds were the pollutants most frequently detected at concentration levels up to 1158ngL−1 (diclofenac).

scholarly journals An Optimized High Throughput Clean-Up Method Using Mixed-Mode SPE Plate for the Analysis of Free Arachidonic Acid in Plasma by LC-MS/MS

2015 ◽  
Vol 2015 ◽  
pp. 1-6 ◽  
Author(s):  
Wan Wang ◽  
Suzi Qin ◽  
Linsen Li ◽  
Xiaohua Chen ◽  
Qunjie Wang ◽  
...  
Keyword(s):  
Arachidonic Acid ◽  
High Throughput ◽  
Mixed Mode ◽  
Preparation Method ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Reversed Phase ◽  
Free Arachidonic Acid

A high throughput sample preparation method was developed utilizing mixed-mode solid phase extraction (SPE) in 96-well plate format for the determination of free arachidonic acid in plasma by LC-MS/MS. Plasma was mixed with 3% aqueous ammonia and loaded into each well of 96-well plate. After washing with water and methanol sequentially, 3% of formic acid in acetonitrile was used to elute arachidonic acid. The collected fraction was injected onto a reversed phase column at 30°C with mobile phase of acetonitrile/water (70 : 30, v/v) and detected by LC-MS/MS coupled with electrospray ionization (ESI) in multiple reaction monitoring (MRM) mode. The calibration curve ranged from 10 to 2500 ng/mL with sufficient linearity (r2= 0.9999). The recoveries were in the range of 99.38% to 103.21% with RSD less than 6%. The limit of detection is 3 ng/mL.

HPLC/Tandem Mass Spectrometric Studies on Steroidal Saponins: An Example of Quantitative Determination of Shatavarin IV from Dietary Supplements Containing Asparagus racemosus

2014 ◽  
Vol 97 (6) ◽  
pp. 1497-1502 ◽  
Author(s):  
Dada Patil ◽  
Manish Gautam ◽  
Sunil Gairola ◽  
Suresh Jadhav ◽  
Bhushan Patwardhan
Keyword(s):  
Acetic Acid ◽  
Dietary Supplements ◽  
Quantitative Estimation ◽  
Multiple Reaction Monitoring ◽  
Asparagus Racemosus ◽  
Steroidal Saponin ◽  
Esi Ms ◽  
Tandem Mass Spectrometric ◽  
Positive Ion

Abstract Asparagus racemosus (AR) is a popular botanical present in several Ayurvedic medicines and nutritional and dietary supplements with immunomodulatory, galactogogue, and anticancer activity. A steroidal saponin known as shatavarin IV is one of the active constituents of AR. A new, selective, and rapid HPLC/MS/MS method has been developed and validated for quantitative estimation of shatavarin IV in crude, processed, and marketed samples of AR. The analytes were separated on a Luna C18 column using simple isocratic elution with water (0.1% acetic acid)–acetonitrile (0.1% acetic acid; 70 + 30, v/v) at a flow rate of 0.8 mL/min. The analytes were detected by electrospray ionization (ESI)-MS/MS and quantified using multiple reaction monitoring techniques in the positive ion mode. The method showed excellent linearity (r2 &gt; 0.998) over the concentration range of 7.5 to 254 ng/mL with LOD of 2.5 ng/mL. Precision (RSD) and accuracy (recovery) were found in the ranges of 2.00 to 5.15 and 102 to 110%, respectively. The validated HPLC/ESI-MS/MS method was successfully applied to the quantification of shatavarin IV in crude, processed, and marketed (single or multiherb) AR samples. Therefore, this method could be used for QC and standardization of pharmaceutical or nutritional products containing AR.

Simultaneous Determination of Four Herbicide and Pesticide Residues in Chinese Green Tea Using QuEChERS Purification Procedure and UPLC-MS/MS Analysis

2013 ◽  
Vol 634-638 ◽  
pp. 1586-1590
Author(s):  
Su Fang Wang ◽  
Shou Jie Zhang ◽  
Chun Hong Dong ◽  
Guo Qing Wang ◽  
Jun Feng Guo ◽  
...  
Keyword(s):  
Formic Acid ◽  
Simultaneous Determination ◽  
Green Tea ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Graphitized Carbon Black ◽  
Ms Analysis ◽  
Relative Standard ◽  
Limit Of Quantitation

A method for simultaneous determination of residuals of four herbicides and pesticides, simazine, carboxin, diflubenzuron and rotenone, in Chinese green tea was developed. In the proposed method, the tea powder was placed in a centrifuge tube with a plug, extracted in saturated aqueous sodium chloride solution and acetonitrile, agitated using vortex oscillator, and then centrifuged 5 min at 4000 rpm. The supernatant solution was purified by primary secondary amine (PSA) sorbent, C18 power, and graphitized carbon black powder, respectively. Then the purified extracts were dissolved with acetonitrile:0.1% formic acid aqueous solution (40:60, V/V) and agitated, filtered using a syringe with 0.22 μm nylon filter prior to UPLC-MS/MS analysis. The UPLC analysis was performed on an ACQUITY UPLC® HSS T3 column (2.1 mm×100 mm, 1.8 µm), using acetonitrile-0.1% formic acid as mobile phase with the flow rate as 0.3 mL•min-1. Injection volume was 10 µL. Positive ionization mode was applied, and the ions were monitored in the multiple reaction monitoring (MRM) mode with curtain gas 0.069 MPa, collision gas 0.052 MPa, ESI ion spray voltage 5000 V, temperature 550 °C, nebulizer gas 0.24 MPa, and turbo gas 0.28 MPa. The limit of detection (LOD) and limit of quantitation (LOQ) of the proposed method are 1 μg•kg-1and 5 μg•kg-1, respectively. The average recoveries of the four pesticides at 10, 20, and 50 µg•kg-1spiking levels range from 77.4% to 95.3%. TheSupersSuperscript textcript textrelative standard deviation (RSD) (n=6) range form 11.83% to 4.52%.

scholarly journals Determination of 77 Multiclass Pesticides and Their Metabolitesin Capsicum and Tomato Using GC-MS/MS and LC-MS/MS

Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 1837
Author(s):  
Harischandra Naik Rathod ◽  
Bheemanna Mallappa ◽  
Pallavi Malenahalli Sidramappa ◽  
Chandra Sekhara Reddy Vennapusa ◽  
Pavankumar Kamin ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Graphitized Carbon Black ◽  
Limit Of Quantification ◽  
Gas And Liquid Chromatography ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Primary Secondary Amine

A quick, sensitive, and reproducible analytical method for the determination of 77 multiclass pesticides and their metabolites in Capsicum and tomato by gas and liquid chromatography tandem mass spectrometry was standardized and validated. The limit of detection of 0.19 to 10.91 and limit of quantification of 0.63 to 36.34 µg·kg−1 for Capsicum and 0.10 to 9.55 µg·kg−1 (LOD) and 0.35 to 33.43 µg·kg−1 (LOQ) for tomato. The method involves extraction of sample with acetonitrile, purification by dispersive solid phase extraction using primary secondary amine and graphitized carbon black. The recoveries of all pesticides were in the range of 75 to 110% with a relative standard deviation of less than 20%. Similarly, the method precision was evaluated interms of repeatability (RSDr) and reproducibility (RSDwR) by spiking of mixed pesticides standards at 100 µg·kg−1 recorded anRSD of less than 20%. The matrix effect was acceptable and no significant variation was observed in both the matrices except for few pesticides. The estimated measurement uncertainty found acceptable for all the pesticides. This method found suitable for analysis of vegetable samples drawn from market and farm gates.

Determination of Bendiocarb Insecticide by Reverse Flow Injection Analysis Using a Solid-Phase Reactor Containing Micro PbO2, Nano PbO2 and Grafted SiO2 - PbO2 Immobilized

2020 ◽  
Vol 42 (1) ◽  
pp. 31-31
Author(s):  
Malik H Alaloosh Alamri Malik H Alaloosh Alamri ◽  
Sadeem Subhi Abed and Abdulkareem M A Alsammarraie Sadeem Subhi Abed and Abdulkareem M A Alsammarraie
Keyword(s):  
Flow Injection ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Reverse Flow ◽  
Blue Color ◽  
Wide Range ◽  
Solid Phase Reactor ◽  
Grafted Nanoparticles ◽  
Reverse Flow Injection

Bendiocarb (BEN) is an acutely toxic carbamate insecticide which used in public places and agriculture, it is also effective against a wide range of nuisance and disease vector insects. A new rapid and sensitive reverse flow injection spectrophotometric procedure coupled with on-line solid-phase reactor is designed in this article for the determination of BEN in its insecticidal formulations and water samples, by using three different solid-phase reactors containing bulk PbO2 (B-SPR), PbO2 nanoparticles (N-SPR) and grafted nanoparticles of SiO2-PbO2 (G-SPR) immobilized on cellulose acetate matrix (CA). This method of oxidative coupling is based on alkaline hydrolysis of the BEN pesticide, and then coupled with N,N dimethyl-p-phenylenediamine sulphate (DMPD) to give a blue color product which measured at λmax 675 nm. It worth to mentioned that under optimal conditions, Beer’s law is obeyed in the range of 1-175 μg mL-1 for B-SPR and 0.25-70 μg mL-1 of BEN for both N-SPR and G-SPR respectively within limit of detection (LOD) of 0.931, 0.234 and 0.210 μg mL-1 for B-SPR N-SPR and G-SPR respectively. The surface methodology of the solid phase was also investigated by using atomic force microscopy.

Determination of Potential Genotoxic Impurity, 5-Amino-2-Chloropyridine, in Active Pharmaceutical Ingredient Using the HPLC-UV System

2020 ◽  
Author(s):  
Murat Soyseven ◽  
Rüstem Keçili ◽  
Hassan Y Aboul-Enein ◽  
Göksel Arli
Keyword(s):  
Analytical Method ◽  
High Performance ◽  
Orthophosphoric Acid ◽  
Limit Of Detection ◽  
Detection System ◽  
Active Pharmaceutical Ingredient ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Water Ph

Abstract A novel analytical method, based on high-performance liquid chromatography with a UV (HPLC-UV) detection system for the sensitive detection of a genotoxic impurity (GTI) 5-amino-2-chloropyridine (5A2Cl) in a model active pharmaceutical ingredient (API) tenoxicam (TNX), has been developed and validated. The HPLC-UV method was used for the determination of GTI 5A2Cl in API TNX. The compounds were separated using a mobile phase composed of water (pH 3 adjusted with orthophosphoric acid): MeOH, (50:50: v/v) on a C18 column (150 × 4.6 mm i.d., 2.7 μm) at a flow rate of 0.7 mL min−1. Detection was carried out in the 254 nm wavelength. Column temperature was maintained at 40°C during the analyses and 10 μL volume was injected into the HPLC-UV system. The method was validated in the range of 1–40 μg mL−1. The obtained calibration curves for the GTI compound was found linear with equation, y = 40766x − 1125,6 (R2 = 0.999). The developed analytical method toward the target compounds was accurate, and the achieved limit of detection and limit of quantification values for the target compound 5A2Cl were 0.015 and 0.048 μg mL−1, respectively. The recovery values were calculated and found to be between 98.80 and 100.03%. The developed RP-HPLC-UV analytical method in this research is accurate, precise, rapid, simple and appropriate for the sensitive analysis of target GTI 5A2Cl in model API TNX.

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