A novel and sensitive LC-MS/MS method for the quantitation of ceftiofur in pharmaceutical preparations and milk samples

2020 ◽  
Vol 23 ◽  
Author(s):  
Serkan Levent ◽  
Saniye Özcan ◽  
Aysun Geven ◽  
Nafiz Öncü Can
Keyword(s):  
Quantitative Estimation ◽  
Signal To Noise Ratio ◽  
Multiple Reaction Monitoring ◽  
Pharmaceutical Preparations ◽  
Calibration Method ◽  
Negative Ion ◽  
Cow Milk ◽  
Tandem Mass ◽  
Ionization Source ◽  
Liquid Chromatography Tandem Mass

Introduction:: In the present study, a sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was described for the determination of ceftiofur (CEF) in cow milk and pharmaceutical preparations. CEF is an antibiotic compound, which is commonly used in the treatment of animal diseases such as respiratory system, soft tissue, and foot infections, as well as postpartum acute puerperal metritis. One of the critical features of CEF is its prescription while breastfeeding of cows; in accordance, its quantitative estimation is essential to assess its residual amounts. Methods:: In the method reported herein, after simple protein precipitation using acetonitrile, the pre-treated samples were introduced in to an LC-MS/MS instrument equipped with a Chromolith® High-Resolution RP-18 series HPLC column (100 mm × 4.6 mm from Merck KGaA, Germany). Electrospray ionization was employed as the ionization source in the triplequadrupole tandem mass spectrometer. Results:: For the calibration method using solvent-based standards; LOQ was 3.038 ng/mL, 12.15 ng/mL, and LOD was 1.215 ng/mL and 6.076 ng/mL for ESI+ and ESI- modes, respectively. On the other hand, for the method of matrix-matched standards; LOQ was 1.701 ng/mL, 10.13 ng/mL, and LOD was 0.486 ng/mL and 5.929 ng/mL for ESI+ and ESI- modes, respectively as obtained from signal to noise ratio. Conclusion:: Applicability of both positive and negative ion modes was tested, and the analyte was detected via multiple reaction monitoring. The distorting effects of the milk matrix on the MS ionization and quantitation of CEF were overcome by using matrix-matched calibration for the first time.

scholarly journals UPLC-MS/MS Method for the Determination of 14 Compounds in Rat Plasma and Its Application in a Pharmacokinetic Study of Orally Administered Xiaoyao Powder

Molecules ◽  
2018 ◽  
Vol 23 (10) ◽  
pp. 2514 ◽  
Author(s):  
Mingyue Xu ◽  
Zhanling Xu ◽  
Qingxuan Xu ◽  
Hongyue Zhang ◽  
Mingyang Liu ◽  
...  
Keyword(s):  
Pharmacokinetic Study ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Ultra Performance Liquid Chromatography ◽  
Rat Plasma ◽  
Chinese Herbs ◽  
Tandem Mass ◽  
Ionization Source ◽  
Liquid Chromatography Tandem Mass ◽  
Negative Ionization

Xiaoyao Powder (XYP), a common Chinese medicine, comprises eight traditional Chinese herbs and has been widely used clinically to treat liver damage and mental disorders. An ultra-performance liquid chromatography–tandem mass spectrometry method was developed to investigate the pharmacokinetics of 14 compounds (albiflorin, paeoniflorin, ferulic acid, senkyunolide I, quercetin, isoliquiritigenin, atractylenolide III, ligustilide, atractylenolide II, liquiritin, liquiritigenin, saikosaponin c, glycyrrhizic acid, and saikosaponin a) in XYP. Naringenin was used as the internal standard. The compounds were separated using an ACQUITY UPLCTM BEH C18 column (1.7 μm, 50 × 2.1 mm) with a mobile phase consisting of acetonitrile and 0.1% formic acid in water at a flow rate of 0.3 mL/min. Detection was performed on a triple-quadrupole tandem mass spectrometer using multiple reaction monitoring and an electrospray ionization source in both positive and negative ionization modes. All calibration curves exhibited good linearity (r2 > 0.9974) over the measured ranges. The intra- and inter-day precisions were within 12%, and the accuracy ranged from 89.93% to 106.64%. Extraction recovery and matrix effect results were satisfactory. The method was successfully applied in a pharmacokinetic study of the 14 compounds in rat plasma after the oral administration of XYP.

scholarly journals Simultaneous determination of multi – component mycotoxin in feeds by liquid chromatography – tandem mass spectrometry

2013 ◽  
Vol 57 (4) ◽  
pp. 567-572 ◽  
Author(s):  
Katarzyna Pietruszka ◽  
Bartosz Sell ◽  
Olga Burek ◽  
Henryka Wiśniewska-Dmytrow
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Ion Trap ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Negative Ion ◽  
Tandem Mass ◽  
Penicillium Species ◽  
Liquid Chromatography Tandem Mass

Abstract A multiresidue method for determination and quantification of Fusarium mycotoxins: deoxynivalenol, zearalenone, T-2 toxin, HT-2 toxin, and metabolite of Aspergillus and Penicillium species - ochratoxin A in feeds was described. The method was based on the simultaneous extraction of selected mycotoxins from matrix, followed by liquid chromatography coupled with tandem mass spectrometry using a hybrid triple quadrupole - linear ion trap mass spectrometer with the multiple reaction monitoring in both positive- and negative-ion modes. The method was validated in accordance with the Commision Decision 2002/657/EC requirements. The mean recoveries of mycotoxins from spiked feed samples ranged from 74.6% to 113.9%, whereas limit of detection and quantification ranged from 0.72 to 12.4 μg/kg and 1.86 to 31.7 μg/kg, respectively.

Serum bile acids profiling by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and its application on pediatric liver and intestinal diseases

2020 ◽  
Vol 58 (5) ◽  
pp. 787-797 ◽  
Author(s):  
Xiaowei Fu ◽  
Yi Xiao ◽  
Jamie Golden ◽  
Sizhe Niu ◽  
Christopher P. Gayer
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Bile Acids ◽  
Multiple Reaction Monitoring ◽  
Negative Ion ◽  
Tandem Mass ◽  
Reaction Monitoring ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

AbstractBackgroundA method for bile acid profiling measuring 21 primary and secondary bile acids in serum samples was developed and validated with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Sample preparation included spiking with internal standards followed by protein precipitation, centrifugation, drying under nitrogen gas and reconstitution. Extracted samples were injected onto a Phenomenex Kinetex C18 column (150 × 4.60 mm, 2.6 μm).MethodsData was collected with LC-MS/MS operated in negative ion mode with multiple reaction monitoring (MRM) and single reaction monitoring (SRM). The analytical run time was 12 min.ResultsThe method showed excellent linearity with high regression coefficients (>0.99) over a range of 0.05 and 25 μM for all analytes tested. The method also showed acceptable intra-day and inter-day accuracy and precision. As a proof of concept, the analytical method was applied to patients with neonatal intrahepatic cholestasis caused by citrin deficiency (NICCD), biliary atresia (BA), and necrotizing enterocolitis (NEC), and distinct bile acids profiles were demonstrated.ConclusionsThe method could be poised to identify possible biomarkers for non-invasive early diagnosis of these disorders.

scholarly journals Simultaneous Determination of Flavonoids from Bamboo Leaf Extracts Using Liquid Chromatography-Tandem Mass Spectrometry

2021 ◽  
Author(s):  
Xiabing Li ◽  
Wuqun Tao ◽  
Hang Xun ◽  
Xi Yao ◽  
Jin Wang ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Simultaneous Determination ◽  
Negative Ion ◽  
Tandem Mass ◽  
Bamboo Species ◽  
Chromatography Tandem Mass Spectrometry ◽  
Liquid Chromatography Tandem Mass

AbstractAn analytical method for the simultaneous determination of ten major functional flavonoids (isoorientin, orientin, vitexin, isovitexin, apigenin, luteolin, tricin, quercetin, rutin, and kaempferol) in different bamboo species was developed by liquid chromatography-tandem mass spectrometry. Chromatographic separation was carried out on a reversed-phase C-18 column with acetonitrile and water as the mobile phases. Detection was performed in negative ion electrospray ionization mode using multiple reaction monitoring mode. The correlation coefficients for the calibration curves ranged from 0.9955 to 0.9997. The limit of detection ranged from 1 to 45 ng/ml. The applicability of this analytical approach was confirmed by the successful analysis of real leaf samples of four bamboo species, family Poaceae: Pleioblastus amarus (Keng) Keng f., Phyllostachys glauca McClure, Phyllostachys edullis (Carrière) J.Houz, and Indocalamus latifolius (Keng) McClure. The total flavonoid contents were 3321.09, 3095.96, 4037.33, and 2808.42 mg/kg for P. amarus, P. glauca, P. edullis, and I. latifolius, respectively. Graphical abstract

Determination of Oxadixyl in Wines by Liquid Chromatography-Tandem Mass Spectrometry: Single-Laboratory and Interlaboratory Validation Study

2014 ◽  
Vol 97 (6) ◽  
pp. 1701-1706
Author(s):  
Armen Mirzoian ◽  
Jeffrey R Ammann
Keyword(s):  
Validation Study ◽  
High Throughput Screening ◽  
Multiple Reaction Monitoring ◽  
Direct Injection ◽  
Ionization Source ◽  
Minimal Sample ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Interlaboratory Validation

Abstract A direct injection LC/MS/MS method for the determination of the pesticide oxadixyl in wines was developed and validated. A sample divert valve was used to deliver the fraction that contained oxadixyl to the mass spectrometer's electrospray ionization source. Oxadixyl was monitored and quantitated using two transitions in multiple reaction monitoring mode. The method demonstrated recoveries of 99.2 ± 2.0 and 96.7 ± 5.2% for red and white wines, respectively, a linearity range of 2–20 μg/L, LOD at 0.7 μg/L, LOQ of 2.0 μg/L, and precision values of 8.2% (RSDr) and 6.2% (RSDR). Direct injection of the wine onto a C18 ultra-performance LC column allowed automation and high throughput screening. Benefits of this approach include minimal sample preparation, short (3 min) run times, and the use of matrix-matched calibration standards, which minimize the matrix effect due to interferences from wine phenolics, sugars, and various other components. The method's performance characteristics were not statistically different for white and red wines. An additional interlaboratory validation study involved 12 laboratories and demonstrated good data agreement with HorRat values ranging from 0.23 to 0.52.

scholarly journals Pharmacokinetics of isocorynoxeine in rat plasma after intraperitoneal administration by UPLC–MS/MS

2020 ◽  
Vol 32 (4) ◽  
pp. 260-263
Author(s):  
Haichao Zhan ◽  
Zhen Wei ◽  
Ke Ren ◽  
Shuhua Tong ◽  
Xianqin Wang ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Tandem Mass Spectrometry ◽  
Multiple Reaction Monitoring ◽  
Intraperitoneal Administration ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Rat Plasma ◽  
Tandem Mass ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

Isocorynoxeine is one of the main alkaloids in Chinese medicinal herbs, and has pharmacological activities such as antihypertensive, sedative, anticonvulsant, and neuronal protection. It is an effective component of Uncaria for the treatment of hypertension. In this study, we used a fast and sensitive ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) to detect isocorynoxeine in rat plasma and investigated its pharmacokinetics in rats. Six rats were given isocorynoxeine (15 mg/kg) by intraperitoneal (i.p.) administration. Blood (100 μL) was withdrawn from the caudal vein at 5 and 30 min and 1, 2, 4, 6, 8, 12, and 24 h after administration. Chromatographic separation was achieved using a UPLC BEH C18 column using a mobile phase of acetonitrile–0.1% formic acid with gradient elution. Electrospray ionization (ESI) tandem mass spectrometry in the multiple reaction monitoring (MRM) mode with positive ionization was applied. Intra-day and inter-day precisions (relative standard deviation, %RSD) of isocorynoxeine in rat plasma were lower than 12%. The method was successfully applied in the pharmacokinetics of isocorynoxeine in rats after intraperitoneal administration. The t1/2 of isocorynoxeine is 4.9 ± 2.1 h, which indicates quick elimination.

scholarly journals Determination of Chloramphenicol in Bovine Milk by Liquid Chromatography/Tandem Mass Spectrometry

2003 ◽  
Vol 86 (4) ◽  
pp. 703-706 ◽  
Author(s):  
Lambert K Sørensen ◽  
Tina H Elbæk ◽  
Helga Hansen
Keyword(s):  
Solid Phase ◽  
Atmospheric Pressure Chemical Ionization ◽  
Bovine Milk ◽  
Negative Ion ◽  
Tandem Mass ◽  
Liquid Chromatography Tandem Mass ◽  
Pressure Chemical Ionization ◽  
Pressure Chemical ◽  
Negative Ion Mode

Abstract A rapid confirmatory liquid chromatographic/tandem mass spectrometic method was developed for determination of chloramphenicol in bovine milk. Chloramphenicol was extracted directly from milk by solid-phase extraction on a C18 cartridge. The extract was further cleaned up on neutral aluminium oxide. Three transition products were monitored in negative ion mode after atmospheric pressure chemical ionization. The detection capability related to the transition product of lowest abundance was 0.03 μg/kg. The mean recovery was 90% at levels of 0.1–0.2 μg/kg. The relative repeatability standard deviations were 4.3, 3.8, and 2.8% at levels of 0.1, 0.2, and 1.0 μg/kg, respectively.

Sign in / Sign up

Export Citation Format

Share Document