Fully-Automated SPE Coupled to UPLC-MS/MS Method for Simultaneous Detection of Trace Sulfonamides, Quinolones, and Macrolide antibiotics in Water

2021 ◽  
Author(s):  
Ming Zheng ◽  
Suwen Tang ◽  
Yangyang Bao ◽  
Kevin D Daniels ◽  
Zuo Tong How ◽  
...  
Keyword(s):  
High Performance ◽  
Matrix Effects ◽  
Solid Phase ◽  
Yangtze River Basin ◽  
Pure Water ◽  
Simultaneous Detection ◽  
Sample Volume ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass

Abstract A fully automated solid-phase extraction (SPE) coupled ultra-high-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed for analysis of antibiotics (sulfonamides, quinolones, and macrolide) in water matrices. Sample preparation optimization included the selection of the best SPE material and configuration (HLB disks), sample volume (500−1000 mL water sample (pH = 3)) with a flow rate at 1−2 mL min− 1, and an elution procedure with 2 ⋅ 6 mL methanol, 2 ⋅ 6 mL acetone-methanol (V/V = 1/1). Meanwhile, the parameters for UPLC-MS/S detection of each analyte was optimized, including LC retention time, and MS parameters. The instrumental limits of detection (LOD) and quantification (LOQ) of analytes ranged from 0.01−0.72 µg L− 1 and 0.05−2.39 µg L− 1, respectively, with good linear correlation (R2 > 0.995) and precision (< 9.9%). Matrix spike recoveries ranged between 63.3−99.2% in pure water, 60.8−91.3% in surface water (SW), and 59.9−102.8% in wastewater effluent (WWE) with relative standard deviations (RSD) below 11%. The matrix effects (MEs) observed for most of the analytes were ion suppression (0−25.8%) except for four compounds that had enhancement (0−8.0 %) in SW or WWE. This method can basically meet the needs of trace antibiotic residues detection in waters. Trace levels of sulfonamides, quinolones and macrolides using the developed antibiotic method were below LOQ (BQL) −94.47 ng L− 1 in WWEs and BQL−15.47 ng L− 1 in SW in the lower reaches of the Yangtze River Basin.

scholarly journals The Effect of Tanreqing Injection on the Pharmacokinetics of Sirolimus in Rats

2019 ◽  
Vol 2019 ◽  
pp. 1-7 ◽  
Author(s):  
Feng Zhang ◽  
Liang Sun ◽  
Jianxiu Zhai ◽  
Tianyi Xia ◽  
Wei Jiang ◽  
...  
Keyword(s):  
High Performance ◽  
Room Temperature ◽  
Matrix Effects ◽  
Thaw Cycle ◽  
Relative Standard ◽  
The Matrix ◽  
Freeze Thaw Cycle ◽  
Liquid Chromatography Tandem Mass ◽  
The Stability ◽  
First Time

To evaluate the effect of Tanreqing injection on the pharmacokinetics of sirolimus in rats, a high performance liquid chromatography tandem mass spectrometry method was developed for sirolimus assay in whole blood. Calibration curve of sirolimus was acquired over a concentration ranging from 2.5 to 100 ng/mL with r2= 0.9955. The matrix effects and extraction recoveries of sirolimus ranged from 144% to 152% and from 80% to 96%, respectively. The inter- and intraday relative standard deviations were both <10%. The stability investigation showed that the blood samples were stable for 30-day-storage at -20°C, for 8 h storage at room temperature, for 24 h storage in the auto-sampler at 4°C, and for three freeze-thaw cycle process. The pharmacokinetic results demonstrated that the Cmax, AUC, and AUMC of sirolimus in rats (7.5 mg/kg, i.g.) were increased after beincoadministration with Tanreqing Injection at 2.5, 5.0, and 7.5 mL/kg (i.v.), respectively, or at 5 min, 2 h, and 4 h (5.0 mL/kg, i.v.) after SRL dosing, respectively. For the first time, the results proved the herb-drug interaction between Tanreqing Injection and sirolimus and accordingly suggested avoiding concurrent reception of those two drugs for patients.

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.

Rapid and Sensitive Detection of Aflatoxin B1, B2, G1 and G2 in Vegetable Oils Using Bare Fe3O4 as Magnetic Sorbents Coupled with High-Performance Liquid Chromatography with Fluorescence Detection

2020 ◽  
Vol 58 (7) ◽  
pp. 678-685
Author(s):  
Hui-Xian Zhang ◽  
Ping Zhang ◽  
Xiao-Fang Fu ◽  
You-Xiang Zhou ◽  
Xi-Tian Peng
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Vegetable Oil ◽  
Vegetable Oils ◽  
Aflatoxin B1 ◽  
High Performance ◽  
Solid Phase ◽  
Simultaneous Detection ◽  
Fluorescence Detector ◽  
Relative Standard

Abstract This paper reports a simple, sensitive and reliable method for the simultaneous detection of aflatoxin B1, B2, G1 and G2 in vegetable oils. Aflatoxins were extracted by magnetic solid phase extraction followed by high-performance liquid chromatography, then postcolumn photochemical derivatization and finally detected by fluorescence detector. Vegetable oil samples were first diluted with hexane and then commercial bare Fe3O4 nanoparticles were directly employed as sorbents to extract aflatoxins from complex vegetable oil samples, which significantly simplified the procedure of sample preparation and largely improved the sample analysis throughput. The effects of various parameters such as the amount of sorbent, loading, washing and eluting conditions were carefully optimized to improve the extraction efficiencies of aflatoxins. Under the optimal conditions, the limits of detection of four aflatoxins ranged from 0.01 μg/kg to 0.16 μg/kg, and squared regression coefficients (R2) &gt;0.9990 were obtained within the linear range of 0.1–20 μg/kg (except for aflatoxin G2 with 0.5–20 μg/kg). Furthermore, the recoveries spiked at four concentration levels in a blank vegetable oil sample were from 82.6 to 106.2%, with inter- and intraday relative standard deviations &lt;9.8%, indicating good accuracy and precision of the proposed method.

scholarly journals Determination of Residual Triflumezopyrim Insecticide in Agricultural Products through a Modified QuEChERS Method

Foods ◽  
2021 ◽  
Vol 10 (9) ◽  
pp. 2090
Author(s):  
Sung-Min Cho ◽  
Han-Sol Lee ◽  
Ji-Su Park ◽  
Su-Jung Lee ◽  
Hye-Sun Shin ◽  
...  
Keyword(s):  
Analytical Method ◽  
Matrix Effects ◽  
Solid Phase ◽  
Reference Method ◽  
Quechers Method ◽  
Modified Quechers ◽  
Relative Standard ◽  
The Matrix ◽  
Food Commodities

A rapid and simple analytical method for triflumezopyrim, a new class of mesoionic insecticides and commercialized molecules from DuPont, was developed with a modified QuEChERS method. The pH adjustment was used to improve the extraction efficiency of acetonitrile solvent, and dispersive solid-phase extraction was employed for the clean-up process. The five selected food commodities were used to verify the present optimized method, which displayed good linearity with an excellent correlation coefficient (R2 = 0.9992–0.9998) in the 0.003–0.30 mg/kg calibration range. The method limits of detection (LOD) and quantification (LOQ) were determined to be a value of 0.003 and 0.01 mg/kg, respectively. The mean recovery for the triflumezopyrim was in the 89.7–104.3% range. The relative standard deviations were ≤9.8% for intra- (n = 5) and inter-day (n = 15) precisions at concentrations of 0.01, 0.1, and 0.5 mg/kg in the five representative samples. The matrix effect has been calculated to confirm the effect during ionization of the analyte in the UPLC-MS/MS. The matrix effects of the instrumental analysis showed that triflumezopyrim was less susceptible to matrices. The proposed analytical method in this study has effectively improved the accuracy, selectivity, and sensitivity for the determination of triflumezopyrim in agricultural commodities; therefore, it can serve as a reference method for the establishment of maximum residue limits (MRLs).

Single-Laboratory Validation of a Multi-residue Method for Simultaneous Analysis of Multi-class Pesticides in Turmeric by Liquid Chromatography Tandem Mass Spectrometry

2020 ◽  
Author(s):  
Bappa Ghosh ◽  
Arijita Bhattacharyya ◽  
Sandip Hingmire ◽  
Pushpa Aher ◽  
Pradnya Zende ◽  
...  
Keyword(s):  
Matrix Effects ◽  
Solid Phase ◽  
Residue Analysis ◽  
High Throughput Analysis ◽  
Method Performance ◽  
Accuracy And Precision ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Powder Samples ◽  
First Time

Abstract Background For years, turmeric has been used in several cuisines worldwide because of its proven health benefits. However, as its cultivation often involves applications of polar and semi-polar pesticides, their residues might cause health hazards to consumers. The dearth of a validated LC-MS/MS method for the residue analysis of these pesticides in turmeric has warranted the present study. Objective The aim was to develop and validate a multi-residue method for simultaneous determination of multi-class pesticides in turmeric (both rhizome and powder) by LC-MS/MS. Method Both the rhizome and powder samples (1 kg) were soaked in water for 30 min, followed by homogenization. Each homogenate (2 g) was mixed with 10 mL water, and extracted with acetonitrile (10 mL) in the presence of acetic acid and NaCl. The extract was cleaned by using dispersive solid phase extraction (dSPE) with graphitized carbon (5 mg/mL) sorbent. The cleaned extract was measured by LC-MS/MS with a runtime of 20 min. The method was validated on 211 multi-class pesticides. Results The method performance was satisfactory at 10 ng/g and higher levels, in compliance with the SANTE/12682/2019 guidelines. The dSPE cleanup was effective in minimizing the matrix effects. The use of matrix-matched calibrations specific for turmeric powder and rhizome corrected all recoveries within the satisfactory range of 70–120%. The precision -RSDs were &lt;20% for all test pesticides. The Horwitz ratio and measurement uncertainty results were satisfactory as well. Conclusions As the method was convenient, selective, accurate, and repeatable, it is recommended for regulatory and commercial testing purposes. Highlights For the first time, this study reports a validated LC-MS/MS method for the multi-residue analysis of pesticides in turmeric. The method provided a high throughput analysis of multi-class pesticides in turmeric rhizome and powder matrices with satisfactory selectivity, sensitivity, accuracy, and precision. The method performance satisfied the requirements of the SANTE/12682/2019 guidelines, and the method sensitivity complied with the EU-MRL requirements.

scholarly journals Toxicokinetics of 11 Gelsemium Alkaloids in Rats by UPLC-MS/MS

2020 ◽  
Vol 2020 ◽  
pp. 1-13
Author(s):  
Xiuwei Shen ◽  
Jianshe Ma ◽  
Xianqin Wang ◽  
Congcong Wen ◽  
Meiling Zhang
Keyword(s):  
Intravenous Administration ◽  
Matrix Effects ◽  
Scientific Evidence ◽  
Simultaneous Detection ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Sprague Dawley ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Main Components

Gelsemium elegans (Gardn. & Champ.) Benth. is a plant belonging to the genus Gelsemium (family Gelsemiaceae), and its main components are alkaloids. It is a Chinese traditional medicinal plant and notoriously known as a highly toxic medicine. However, a method has not yet been found for the simultaneous detection of 11 Gelsemium alkaloids in rat plasma, and the toxicokinetics of 11 Gelsemium alkaloids after intravenous administration has not been reported. In this work, we have developed a sensitive and rapid method of ultraperformance liquid chromatography/tandem mass spectrometry (UPLC-MS/MS) for the detection of 11 Gelsemium alkaloids in rat plasma. The toxicokinetic behavior was also investigated, so as to provide a reference of the scientific properties of Gelsemium elegans and improve the efficacy and safety of drugs. Sixty-six Sprague-Dawley rats were randomly divided into 11 groups, six rats in each group. Each group was intravenously given one alkaloid (0.1 mg/kg), respectively. A Waters UPLC BEH C18 column (50 mm×2.1 mm, 1.7 μm) was used for chromatographic separation. Methanol and water (containing 0.1% formic acid) were used for the mobile phase with gradient elution. Multiple reactions were monitored, and positive electrospray ionization was used for quantitative analysis. The precision was less than 16%, and the accuracy was between 86.9% and 113.2%. The extraction efficiency was better than 75.8%, and the matrix effects ranged from 88.5% to 107.8%. The calibration curves were in the range of 0.1–200 ng/mL, with a correlation coefficient (R2) greater than 0.995. The UPLC-MS/MS method was successfully applied to the toxicokinetics of 11 Gelsemium alkaloids in rats after intravenous administration (0.1 mg/kg for each alkaloid). The results of the toxicokinetics provide a basis for the pharmacology and toxicology of Gelsemium alkaloids and scientific evidence for the clinical use of Gelsemium alkaloids.

scholarly journals Simultaneous Determination of Five Components of Chaihu-Shugan-San in Beagle Plasma by HPLC-MS/MS and Its Application to a Pharmacokinetic Study after a Single Dose of Chaihu-Shugan-San

2020 ◽  
Vol 2020 ◽  
pp. 1-11
Author(s):  
Yong-liang Zhu ◽  
Hui-jun Wang ◽  
Hao Xue ◽  
Yi Zhang ◽  
Qian-shi Cheng ◽  
...  
Keyword(s):  
Single Dose ◽  
High Performance ◽  
Matrix Effects ◽  
Gradient Elution ◽  
Gastrointestinal Diseases ◽  
Column Temperature ◽  
Mobile Phases ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Total Measurement Time

Chaihu-shugan-san (CHSGS) has been widely used in China to treat depression and gastrointestinal diseases for thousands of years, but little is known about its pharmacokinetic properties. The purpose of our study is to develop a reliable and sensitive high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method to detect five components in beagle plasma and study their pharmacokinetic after oral administration of CHSGS in beagles. An Agilent C18 column (2.1 × 150 mm, 3.5 μm) was used to separate the analytes, and the column temperature was maintained at 40°C. A gradient elution procedure was used with solvent A (acetonitrile) and solvent B (0.1% formic acid, aqueous) as mobile phases. The elution procedure was 60% B—10% B (0–3 min) and 10% B—60% B (3.1–4 min). The flow rate was 0.3 mL/min, and the total measurement time was 4 min. Within the determined range, the standard calibration curves of the five analytes had a satisfactory linear relationship (r2 ≥ 0.9923). The recovery rate (n = 6) of the five analytes was between 85.42% and 90.85%, and the matrix effects (n = 6) were between 94.52% and 103.91%. These results show that the validated method could be successfully applied to study the pharmacokinetic in beagles after a single dose of CHSGS.

Application of a Validated UPLC–MS-MS Method for the Determination of Diphenidol in Biological Samples in 15 Authentic Lethal Cases

2020 ◽  
Author(s):  
Liu Yang ◽  
Min Shen ◽  
Ping Xiang ◽  
Baohua Shen ◽  
Hongxiao Deng ◽  
...  
Keyword(s):  
Biological Samples ◽  
High Performance ◽  
Sample Volume ◽  
Accidental Poisoning ◽  
Antiemetic Drug ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Heart Blood ◽  
Lower Limits

Abstract Diphenidol (DPN) is a nonphenothiazinic antivertigo and antiemetic drug that has been widely used in clinical practice in China because of its good antivertigo curative effect, minimal side effects and high safety. In recent years, there have been some cases of sporadic suicide and accidental poisoning related to DPN. Hence, a validated method for the determination of DPN in biological samples by ultra-high-performance liquid chromatography tandem mass spectrometry (UPLC–MS-MS) was developed. The method is characterized by the use of a simple, fast and inexpensive liquid–liquid extraction (LLE) for sample preparation, a rapid run time (5 min) and a low required sample volume (0.1 mL or 0.1 g). The lower limits of quantitation (LLOQs) were 0.05 ng/mL and 0.3 ng/g for blood and liver tissue, respectively. The method was shown to be linear over a concentration range of 0.05 ∼ 200 ng/mL (blood) and 0.3 ∼ 400 ng/g (liver). The accuracy was in the range of 92.77% ∼ 112.75%. The relative standard deviations of the intraday and interday imprecisions were in the range of 3.22% to 12.17%, and the recoveries were in the range of 58.75% ∼ 95.27%. Furthermore, the method was successfully applied to the detection and quantification of DPN in 15 real forensic cases. The postmortem concentration range of heart blood was 0.87 ∼ 99 μg/mL.

scholarly journals A Rapid Method Based on Hot Water Extraction and Liquid ChromatographyTandem Mass Spectrometry for Analyzing Tetracycline Antibiotic Residues in Cheese

2007 ◽  
Vol 90 (3) ◽  
pp. 864-871 ◽  
Author(s):  
Sara Bogialli ◽  
Cristina Coradazzi ◽  
Antonio Di Corcia ◽  
Aldo Lagana ◽  
Manuel Sergi
Keyword(s):  
Mass Spectrometry ◽  
Extraction Efficiency ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Hot Water ◽  
Phase Dispersion ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
The Mean

Abstract A rapid, specific, and sensitive procedure for determining residues of 4 widely used tetracycline antibiotics and 3 of their 4-epimers in cheese is presented. The method is based on the matrix solid-phase dispersion (MSPD) technique followed by liquid chromatography/tandem mass spectrometry (LC/MS/MS). After dispersing samples of mozzarella, asiago, parmigiano, gruyere, emmenthal, and camembert on sand, target compounds were eluted from the MSPD column by passing through it 6 mL water heated at 70C. After acidification and filtration, 200 L of the aqueous extract was directly injected into the LC column. For analyte identification and quantification, MS data acquisition was performed in the multireaction monitoring mode, selecting 2 precursor ion-to-product ion transitions for each target compound. Hot water appeared to be an efficient extractant, because absolute recoveries were no lower than 78%. Using demeclocycline as a surrogate analyte, recoveries of analyte added to the 6 types of cheeses at the 30 ng/g level were 96117%, with relative standard deviation (RSD) not higher than 9%. Statistical analysis of the mean recovery data showed that the extraction efficiency was not dependent on the type of cheese analyzed. This result indicates that this method could be applied to other cheese types not considered here. At the lowest concentration considered, i.e., 10 ng/g, the accuracy of the method ranged between 90 and 107%, with RSDs not larger than 12%. Based on a signal-to-noise ratio of 10, limits of quantitation were estimated to be 12 ng/g.

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