scholarly journals Determination of Polypeptide Antibiotic Residues in Food of Animal Origin by Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry

Molecules ◽  
2020 ◽  
Vol 25 (14) ◽  
pp. 3261
Author(s):  
Tomasz Bladek ◽  
Iwona Szymanek-Bany ◽  
Andrzej Posyniak
Keyword(s):  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Animal Origin ◽  
Antibiotic Residues ◽  
Triple Quadrupole Mass Spectrometer ◽  
Limit Of Quantification ◽  
Food Of Animal Origin ◽  
Polypeptide Antibiotic

A novel UHPLC-MS/MS method for the determination of polypeptide antibiotic residues in animal muscle, milk, and eggs was developed and validated. Bacitracin A, colistin A, colistin B, polymyxin B1, and polymyxin B2 were extracted from the samples with a mixture of acetonitrile/water/ammonia solution 25%, 80/10/10 (v/v/v), and put through further evaporation, reconstitution, and filtration steps. The chromatographic separation was performed on a C18 column in gradient elution mode. Mass spectral acquisitions were performed in selective multiple reaction monitoring mode by a triple quadrupole mass spectrometer. The method was validated according to the criteria of Commission Decision 2002/657/EC. The method quantifies polypeptides in a linear range from 10 to 1000 μg kg−1, where the lowest concentration on the calibration curve refers to the limit of quantification (LOQ). The recoveries ranged from 70 to 99%, the repeatability was below 13%, and within-laboratory reproducibility was lower than 15%. The decision limit (CCα) and detection capability (CCβ) values were calculated, and ruggedness and stability studies were performed, to fulfill the criteria for confirmatory methods. Moreover, the developed method may also be used for screening purposes by its labor efficiency.

Simultaneous Determination of Eight Potential Q-Markers in Zishen Tongguan Capsules Based on UHPLC-MS/MS

2020 ◽  
Vol 17 (1) ◽  
pp. 47-56
Author(s):  
Shun Liu ◽  
Xun Wang ◽  
Kaiping Zou ◽  
Wei Liu ◽  
Cunyu Li ◽  
...  
Keyword(s):  
Quality Control ◽  
Chinese Medicine ◽  
Simultaneous Determination ◽  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Quality Markers ◽  
High Repeatability ◽  
Comprehensive Study

Background: Zishen Tongguan (ZSTG) capsules were prepared at the Affiliated Hospital of Nanjing University of Chinese Medicine and have been proven to be clinically effective for treating pyelonephritis and benign prostatic hyperplasia. However, the quality standards are not ideal; a comprehensive study of the “quality markers” (Q-markers), the chemicals inherent in traditional Chinese medicine and its preparations, has not been carried out. Experimental Methods: In this paper, a sensitive and specific ultra-high-performance liquid chromatographictandem mass spectrometry (UHPLC-MS/MS) method was developed for the simultaneous determination of eight potential Q-markers of ZSTG, including timosaponin A3, berberine, jatrorrhizine, phellodendrine, palmatine, mangiferin, neomangiferin, and timosaponin BII. A Kromasil 100-3.5 C18 column was used with a mobile phase of 0.2% formic acid with acetonitrile, and gradient elution at a flow rate of 0.2 mL/min was achieved in 13 minutes and used for separation. Detection was performed in positive/negative mode with multiple reaction monitoring (MRM). Results: The analytical method was validated in terms of the sensitivity, linearity, accuracy, precision, repeatability, stability and recovery. The method established here was successfully applied to study the potential Q-markers in 8 batches of commercial samples, which demonstrated its use in improving the quality control of ZSTG. Conclusion: The developed method had high repeatability and accuracy and was suitable for the simultaneous analysis of multiple Q-markers, which may provide a new basis for the comprehensive assessment and overall quality control of ZSTG.

scholarly journals UHPLC-QQQ-MS/MS assay for quantification of dianthrones as potential toxic markers of Polygonum multiflorum Thunb: Application to the standardization of TCMs with endogenous toxicity

2021 ◽  
Author(s):  
Jian-Bo Yang ◽  
Yun-Fei Song ◽  
Yue Liu ◽  
Hui-Yu Gao ◽  
Qi Wang ◽  
...  
Keyword(s):  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Triple Quadrupole ◽  
Quadrupole Mass ◽  
Polygonum Multiflorum ◽  
Triple Quadrupole Mass Spectrometer ◽  
Benefit Risk Assessment ◽  
Heparg Cells

Abstract Background: The raw and processed roots of Polygonum multiflorum Thunb (PM) are commonly used in clinical practice to treat diverse diseases; however, the reports of hepatotoxicity induced by Polygoni Multiflori Radix (PMR) and Polygoni Multiflori Radix Praeparata (PMRP) have emerged worldwide. Thus, it is necessary for researcher to explore the methods to improve its quality standards and further ensure its quality and treatment effect.Methods: In the present study, an ultra-high-performance liquid chromatography coupled with triple quadrupole mass spectrometry (UHPLC-QQQ- MS/MS) method has been optimized and validated for the determination of dianthrones in PMR and PMRP, using bianthronyl as the internal standard. Chromatographic separation with a gradient mobile phase (A: acetonitrile and B: water containing 0.1% formic acid (v/v)) at a flow rate of 0.25 mL/min was achieved on a Waters Acquilty UPLC BEH b) C18 column (2.1 mm × 50 mm, 1.7 µm). A triple quadrupole mass spectrometer (TQMS) was operated in negative ionization mode with multiple reaction monitoring for the quantitative analysis of six dianthrones. Meanwhile, compounds 5 and 6 were further evaluated for cytotoxicity of HepaRG cells by CCK8 assay.Results: The UHPLC-QQQ-MS/MS method was first developed to simultaneous determination of six dianthrones in PMR and PMRP, namely polygonumnolides C1–C4 (1–4), trans-emodin dianthrones (5), and cis-emodin dianthrones (6). The contents of 1~6 in 90 batches of PMR were in the range of 0.027-19.04, 0.022-13.86, 0.073 -15.53, 0.034 -23.35, 0.38-83.67 and 0.29 -67.00 µg/g, respectively. The contents of 1~6 in 86 batches of commercial PMRP were in the range of 0.020-13.03, 0.051-8.94, 0.022-7.23, 0.030 -12.75, 0.098-28.54 and 0.14-27.79 µg/g, respectively. The six dianthrones were almost completely gone after reasonable processing for 24 h. Meanwhile, compounds 5 and 6 showed the inhibitory activity against HepaRG cells with the IC50 values of 10.98 and 15.45 μM, respectively. Furthermore, a systematic five-step strategy to realize the standardization of TCMs with endogenous toxicity is proposed for the first time, involving the establishment of determination methods, determination of the toxic markers, the standardization of processing method, the development of limit standards and benefit-risk assessment.Conclusion: The results of cytotoxicity evaluation of dianthrone indicated that trans-emodin dianthrones (5) and cis-emodin dianthrones (6) could be selected as the toxic markers of PMRP. Taking PMR and PMRP for example, we hope this study provided insight into the standardization and internationalization of endogenous toxic TCMs, with the main purpose of improving public health by scientifically using TCMs to treat diverse complex diseases in future.

scholarly journals A Simple High-Performance Liquid Chromatography Method for Simultaneous Determination of Three Triazole Antifungals in Human Plasma

2012 ◽  
Vol 57 (1) ◽  
pp. 484-489 ◽  
Author(s):  
Mei Zhang ◽  
Grant A. Moore ◽  
Murray L. Barclay ◽  
Evan J. Begg
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Human Plasma ◽  
High Performance ◽  
Internal Standard ◽  
Gradient Elution ◽  
Limit Of Quantification ◽  
Chromatography Method

ABSTRACTA rapid and simple high-performance liquid chromatography (HPLC) assay was developed for the simultaneous determination of three triazole antifungals (voriconazole, posaconazole, and itraconazole and the metabolite of itraconazole, hydroxyitraconazole) in human plasma. Sample preparation involved a simple one-step protein precipitation with 1.0 M perchloric acid and methanol. After centrifugation, the supernatant was injected directly into the HPLC system. Voriconazole, posaconazole, itraconazole, its metabolite hydroxyitraconazole, and the internal standard naproxen were resolved on a C6-phenyl column using gradient elution of 0.01 M phosphate buffer, pH 3.5, and acetonitrile and detected with UV detection at 262 nm. Standard curves were linear over the concentration range of 0.05 to 10 mg/liter (r2> 0.99). Bias was <8.0% from 0.05 to 10 mg/liter, intra- and interday coefficients of variation (imprecision) were <10%, and the limit of quantification was 0.05 mg/liter.

scholarly journals Multiresidue method for the simultaneous analysis of antibiotics and mycotoxins in feeds by ultra-high performance liquid chromatography coupled to tandem mass spectrometry

2021 ◽  
Author(s):  
Ü.İ. Konak ◽  
H.A. Yatmaz ◽  
Ş. Nilüfer ◽  
T. Erkaymaz ◽  
M. Certel
Keyword(s):  
High Performance ◽  
Safety Issue ◽  
Animal Health ◽  
Animal Origin ◽  
Limit Of Quantification ◽  
Multiresidue Method ◽  
Animal Feeds ◽  
Relative Standard ◽  
Feed Samples

AbstractResidues in animal feeds and foods of animal origin have been important safety issue concerning both human and animal health. A multiresidue method for determination of eight mycotoxins and ten antibiotics was developed and validated in animal feeds by using QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction followed by UHPLC-MS/MS. Optimisation of UHPLC-MS/MS parameters was performed to achieve good separation and resolution. The method was validated according to the European Commission Decision 2002/657/EC. Matrix matched calibration curves showed good r2 (≥0.995) values, and limit of quantification (LOQ) values varied between 1.2 and 5.2 μg kg−1. Average recoveries ranged from 60 to 102% with relative standard deviations of 2.2 and 15.6% for all type of feed samples except for tetracyclines, lincomycin, tylosin, ochratoxin A, and fumonisin (B1 and B2).

Determination of ephedrine, pseudoephedrine, sinapine thiocyanate, tetrahydropalmatine and amygdalin by HPLC-MS/MS after oral administration of extracts of Majie cataplasm in rabbits plasma: Application to a pharmacokinetic study

2020 ◽  
Author(s):  
Changxiang Li ◽  
Hanfen Shi ◽  
Fafeng Cheng ◽  
Wenxiang Zhu ◽  
Yuanjun Liu ◽  
...  
Keyword(s):  
Oral Administration ◽  
Pharmacokinetic Study ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Limit Of Quantification ◽  
Chromatographic Separations ◽  
Qualitative Detection ◽  
Chromatographic Resolution ◽  
First Time

Abstract BackgroundThis study aimed to develop HPLC-MS/MS method for quantification of ephedrine, pseudoephedrine, sinapine thiocyanate, tetrahydropalmatine and amygdalin of extracts of Majie cataplasm after oral administration in rabbits plasma and describe the pharmacokinetics of this five components.MethodsThe qualitative detection of the five compounds was accomplished by two methods. One method for the simultaneous determination of ephedrine, pseudoephedrine, sinapine thiocyanate and tetrahydropalmatine was developed and validated for the first time, while the other method was for amygdalin. Chromatographic separations were achieved on a C18 column using gradient elution with the mobile phase consisting of acetonitrile and water (containing 0.1% formic acid and 5mM ammonium formate) for ephedrine, pseudoephedrine, sinapine thiocyanate and tetrahydropalmatine, while acetonitrile and water for amygdalin, at a flow rate of 0.4 mL/min. The initial gradient was extended in order to isolate ephedrine and pseudoephedrine better. The detection was performed in multiple-reaction monitoring (MRM) mode using electrospray ionization (ESI).ResultsAll calibration curves showed good linearity (r2＞0.996) within the test ranges. The lower limit of quantification was 0.01 ng/mL for all five analytes. Reproducibility for five analytes ranged from 0.79 to 2.3% (Ephedrine), 0.51 to 3.4% (pseudoephedrine), 2.8 to 5.0% (Sinapine thiocyanate), 2.6 to 6.3% (Tetrahydropalmatine) and 1.1—2.5% (amygdalin) respectively. The extraction recoveries were within the acceptable range.ConclusionThe two methods were successfully applied to pharmacokinetic study of rabbits after oral administration. The two methods has several advantages including good chromatographic resolution, specific and reproducibility and superior minimum detection limit. The results provided a basis for further study on the bioactivity of Majie cataplasm.

scholarly journals Determination of 5-nitro-2-furaldehyde as marker residue for nitrofurazone treatment in farmed shrimps and with addressing the use of a novel internal standard

2019 ◽  
Vol 9 (1) ◽  
Author(s):  
Qiang Wang ◽  
Xu-Feng Wang ◽  
Yong-Yuan Jiang ◽  
Zhi-Guang Li ◽  
Nan Cai ◽  
...  
Keyword(s):  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Gradient Elution ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Negative Ionization ◽  
Ultrasonic Manipulation

AbstractWe developed a significantly improved ultra-high performance liquid chromatography-tandem mass spectrometry method for determination of 5-nitro-2-furaldehyde (NF) as a surrogate using a novel internal standard for the detection of nitrofurazone. We used 2,4-dinitrophenylhydrazine derivatization and furfural as the internal standard. Derivatization was easily performed in HCl using ultrasonic manipulation for 5 min followed by liquid extraction using ethyl acetate. The samples were concentrated and purified using reverse phase and alumina cartridges in tandem. The derivatives were separated using a linear gradient elution on a C18 column with methanol and water as the mobile phase in negative ionization mode and multiple reaction monitoring. Under the optimized conditions, the calibration curves were linear from 0.2 to 20 μg/L with correlation coefficients >0.999. Mean recoveries were 80.8 to 104.4% with the intra- and inter-day relative standard deviations <15% at spiking levels of 0.1 to 10 μg/kg. The limits of detection and quantification were 0.05 and 0.1 μg/kg, respectively. This method is a robust tool for the identification and quantitative determination of NF in shrimp samples.

A UPLC-MS/MS Assay for Simultaneous Determination of Two Antipsychotics and Two Antidepressants in Human Plasma and Its Application in Clinic

2020 ◽  
Vol 21 (1) ◽  
pp. 60-69
Author(s):  
Houli Li ◽  
Xiaoliang Cheng ◽  
Di Zhang ◽  
Maoyi Wang ◽  
Weihua Dong ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Human Plasma ◽  
High Performance ◽  
Medication Compliance ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Individual Therapy ◽  
Therapeutic Drug ◽  
Ionization Source

Background: Antidepressants and antipsychotics are widely prescribed drugs for the treatment of mental diseases. Therapeutic drug monitoring (TDM) is recommended for patients taking these drugs to ensure pharmaceutical efficacy, medication compliance and prevent toxicity. Objective: An ultra-high performance liquid chromatography/tandem-mass spectrometry (UPLC-MS/ MS) method was developed for simultaneous determination of two Antidepressants-Fluoxetine (FLU) and Escitalopram (ESC), and two antipsychotics-risperidone (RIS) and aripiprazole (ARI), in human plasma. Methods: The sample was processed by simple protein precipitation and the targeted analytes were separated on a C18 column by gradient elution with a mobile phase containing 0.1% formic acid (v/v) and acetonitrile. All the analytes were qualitative and quantitative measured by electrospray ionization source with Multiple Reaction Monitoring (MRM) in positive ion mode. A total of 56 plasma samples were obtained from out- or in-patients who were taking the cited four drugs for further analysis. Results: The calibration curves for FLU, ESC, RIS and ARI were linear in the range of 45-1800, 4-320, 2-200 and 50-1800 ng/mL, respectively. The entire analytical time for the analytes was 7.0 min for each run and the extraction efficiency was more than 90%. The sample was stable within various storage conditions. The trough concentrations in patients were measured with the validated method. Conclusions: The developed method was successfully used for simultaneous determination of FLU, ESC, RIS and ARI in the plasma of the patients, which provides effective technical support for routine TDM of these four drugs and is of great clinic value for individual therapy.

scholarly journals Determination of Tranquilizers in Swine Urine by Ultra-High-Performance Liquid Chromatography-Tandem Mass Spectrometry

Molecules ◽  
2018 ◽  
Vol 23 (12) ◽  
pp. 3215 ◽  
Author(s):  
Yingyu Wang ◽  
Xiaowei Li ◽  
Yuebin Ke ◽  
Chengfei Wang ◽  
Yuan Zhang ◽  
...  
Keyword(s):  
High Performance ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Single Step ◽  
Swine Urine ◽  
Relative Standard ◽  
Positive Mode

A rapid, reliable, and sensitive method was developed for the determination of ten tranquilizers in swine urine. Sample preparation was based on solid-phase extraction, which combined isolation of the compounds and sample cleanup in a single step. Separation was performed on a reversed phase C18 column by gradient elution with a chromatographic run time of seven minutes, consisting of 0.1% formic acid in water and acetonitrile as the mobile phase. Multiple reaction monitoring in positive mode was applied for data acquisition. Matrix-matched calibration was used for quantification and good linearity was obtained with coefficients of determination higher than 0.99. The average recoveries of fortified samples at concentrations between 0.05 and 10 µg/L ranged from 85% to 106% with interday relative standard deviations of less than 13% in all cases. The limits of detection and limits of quantification obtained for tranquilizers in the urine were in the ranges of 0.03–0.1 µg/L and 0.05–0.25 µg/L, respectively. The applicability of the proposed method was demonstrated by analyzing real samples; diazepam was detected at concentrations between 0.3 and 0.6 μg/L.

scholarly journals Simultaneous determination of some illegal antihypertensive and diuretic drugs in traditional herbal preparations by HPLC-DAD

2021 ◽  
Vol 4 (2) ◽  
pp. 99-108
Author(s):  
Hung Pham Van ◽  
Son Tran Cao ◽  
Kieu Anh Nguyen Thi ◽  
◽  
◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Gradient Elution ◽  
Local Market ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Herbal Products ◽  
Herbal Preparations ◽  
Diuretic Drugs

A simple, stable, and specific high-performance liquid chromatography coupled with a&nbsp;DAD detector (HPLC-DAD) method has been developed and validated for the simultaneous&nbsp;determination of amlodipine, felodipine, furosemide, nifedipine, and spironolactone in&nbsp;traditional herbal products. The analytes were extracted in acetonitrile: water (50 : 50, v/v) with&nbsp;help of the ultrasonic. The separation of analytes was performed in an Apollo C18 column (250&nbsp;&times; 4.6 mm; 5 &mu;m) and a mobile phase consisting of mixture acetonitrile: 0.1% phosphoric acid in&nbsp;gradient elution. The analyzed drugs were detected at 238 nm. The method was validated according&nbsp;to the AOAC International guidelines concerning specificity, linearity, precision (repeatability,&nbsp;intermediate precision), accuracy, limit of detection (LOD), and limit of quantification (LOQ).&nbsp;The method can detect the studied drugs at the concentration of 0.66 to 1.25 &mu;g/g for dry&nbsp;samples and 0.10 to 0.24 &mu;g/mL for liquid samples. The method was successfully applied in the&nbsp;analysis of 17 samples in the local market. No samples were found positive for the substances to&nbsp;be analyzed.

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