scholarly journals An Established HPLC-MS/MS Method for Evaluation of the Influence of Salt Processing on Pharmacokinetics of Six Compounds in Cuscutae Semen

Molecules ◽  
2019 ◽  
Vol 24 (13) ◽  
pp. 2502 ◽  
Author(s):  
Jiao Liu ◽  
Shuhan Zou ◽  
Wei Liu ◽  
Jin Li ◽  
Hui Wang ◽  
...  
Keyword(s):  
Chlorogenic Acid ◽  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Negative Ion ◽  
Coumaric Acid ◽  
Liquid Chromatography Mass Spectrometry ◽  
Pharmacokinetic Properties ◽  
Neochlorogenic Acid ◽  
Negative Ion Mode ◽  
Lower Limits

A sensitive and effective method was developed for clarifying the pharmacokinetic properties of six compounds (including hyperin, chlorogenic acid, neochlorogenic acid, p-coumaric acid, astragalin, and isoquercitrin) in two processed Cuscutae Semen samples by high performance liquid chromatography mass spectrometry (HPLC-MS/MS). The six compounds were separated by acetonitrile and 0.1% formic acid-water on an Agilent Eclipse plus C18 column (4.6 mm × 100 mm, 1.8 μm). All compounds were analyzed with negative ion mode in multiple reaction monitoring (MRM). The lower limits of quantification (LLOQ) of hyperin, astragalin, neochlorogenic acid, chlorogenic acid, isoquercitrin, and p-coumaric acid were 1, 0.1, 4, 0.1, 2, and 4 ng·mL−1, respectively. The validated approach was effectively used for the pharmacokinetics of six compounds of two processed Cuscutae Semen samples after oral administration to rat. The results indicated that salt processing could improve the adsorption and bioavailability of astragalin in Cuscutae Semen.

UHPLC-MS Simultaneous Determination and Pharmacokinetic Study of Three Aromatic Acids and One Monoterpene in Rat Plasma after Oral Administration of Shaofu Zhuyu Decoction

2013 ◽  
Vol 41 (03) ◽  
pp. 697-715 ◽  
Author(s):  
Shulan Su ◽  
Wenxia Cui ◽  
Jin-Ao Duan ◽  
Yongqing Hua ◽  
Jianming Guo ◽  
...  
Keyword(s):  
Oral Administration ◽  
Pharmacokinetic Study ◽  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Rat Plasma ◽  
Negative Ion ◽  
Aromatic Acids ◽  
Active Components ◽  
Negative Ion Mode

We developed a sensitive and rapid method for determination of ferulic acid, caffeic acid, vanillic acid, and paeoniflorin in rat plasma based on ultra high performance liquid chromatography coupled with tandem mass spectrometry (UHPLC–MS/MS). The separation of the four compounds was carried out on an AcQuity UHPLC™ BEH C18 column using a mobile phase consisting of acetonitrile and water (containing 0.1% formic acid). Electrospray ionization in positive and negative ion mode and multiple reaction monitoring was used to identify and quantify active components. All calibration curves gave good linearity (r > 0.991) over the concentration range from 4.24–2875 ngmL-1 for all components. The precision of the in vivo study was evaluated by intraday and interday assays and the percentages of RSD were all within 10.6%. The recovery ranged from 60.2 to 77.9%. The method was successfully applied to pharmacokinetic study of all three aromatic acids and one monoterpene in rat plasma. Furthermore, we compared the pharmacokinetics profile of the four compounds in normal and primary dysmenorrhea rats' plasma following oral administration of Shaofu Zhuyu decoction (SFZYD) and its ethanol supernatant extract (SFE).

scholarly journals A Mass Spectrometry-Based Approach for Characterization of Red, Blue, and Purple Natural Dyes

Molecules ◽  
2020 ◽  
Vol 25 (14) ◽  
pp. 3223
Author(s):  
Katarzyna Lech ◽  
Emilia Fornal
Keyword(s):  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Natural Dyes ◽  
Negative Ion ◽  
Near Eastern ◽  
Esi Ms ◽  
Historical Objects ◽  
Tandem Mass Spectrometric ◽  
Negative Ion Mode ◽  
Analytical Approaches

Effective analytical approaches for the identification of natural dyes in historical textiles are mainly based on high-performance liquid chromatography coupled with spectrophotometric detection and tandem mass spectrometric detection with electrospray ionization (HPLC-UV-Vis-ESI MS/MS). Due to the wide variety of dyes, the developed method should include an adequate number of reference color compounds, but not all of them are commercially available. Thus, the present study was focused on extending of the universal analytical HPLC-UV-Vis-ESI MS/MS approach to commercially unavailable markers of red, purple, and blue dyes. In the present study, HPLC-UV-Vis-ESI MS/MS was used to characterize the colorants in ten natural dyes (American cochineal, brazilwood, indigo, kermes, lac dye, logwood, madder, orchil, Polish cochineal, and sandalwood) and, hence, to extend the analytical method for the identification of natural dyes used in historical objects to new compounds. Dye markers were identified mostly on the basis of triple quadrupole MS/MS spectra. In consequence, the HPLC-UV-Vis-ESI MS/MS method with dynamic multiple reaction monitoring (dMRM) was extended to the next 49 commercially unavailable colorants (anthraquinones and flavonoids) in negative ion mode and to 11 (indigoids and orceins) in positive ion mode. These include protosappanin B, protosappanin E, erythrolaccin, deoxyerythrolaccin, nordamnacanthal, lucidin, santalin A, santalin B, santarubin A, and many others. Moreover, high-resolution QToF MS data led to the establishment of the complex fragmentation pathways of α-, β-, and γ- aminoorceins, hydroxyorceins, and aminoorceinimines extracted from wool dyed with Roccella tinctoria DC. The developed approach has been tested in the identification of natural dyes used in 223 red, purple, and blue fibers from 15th- to 17th-century silk textiles. These European and Near Eastern textiles have been used in vestments from the collections of twenty Krakow churches.

scholarly journals Chromatography-tandem MASS spectrometry (HPLC-MS/MS) for the detection of valproic acid and its metabolites in blood plasma

2018 ◽  
Vol 10 (2) ◽  
pp. 35-42
Author(s):  
A. S. Malygin ◽  
N. S. Popov ◽  
M. A. Demidova ◽  
M. N. Kudrayshova
Keyword(s):  
Valproic Acid ◽  
Blood Plasma ◽  
Ammonium Acetate ◽  
Therapy Monitoring ◽  
Multiple Reaction Monitoring ◽  
Negative Ion ◽  
The Individual ◽  
Negative Ion Mode ◽  
Patients With Epilepsy ◽  
In Blood Plasma

Aim: to adapt the HPLC-MS/MS technique to determining valproic acid and its metabolites in blood plasma for drug therapy monitoring.Materials and Methods: The chromatographic assay was run using an Agilent 1260 Infinity II chromatograph with a Phenomenex synergi Fusion analytical column 4 μm-C18 2×50 mm. The mobile phase consisted of 0.1% ammonium acetate in distilled water and 0.1% ammonium acetate in methanol (10:90 v/v, 0.5 ml/min). The multiple ions monitoring (MIM) mode was used for mass- spectrometric detection of valproic acid at m/z = 143.1, with the negative ion mode. The method  was found applicable over the range from 1 mcg/ml to 200 mcg/ml of valproic acid. For the mass  spectroscopy detection of valproic acid metabolites, the multiple reaction monitoring (MRM mode)  was used. MS identifications of 2-propyl-4-pentanoil-β-О-glucuronide; 2-propyl-4-pentenoic acid,  3-hydroxy-2- propylpentanoic acid, 4-hydroxy-2-propylpentanoic acid, 2-propylglutaric acid and 3- oxo-2-propylpentanoic acid in the negative ion mode were carried out at m/z 319.2→143.2; m/z  140.1→140.1; m/z 159.1→101; m/z 159.1→123.1; m/z 173→129.1 and m/z 157.05→11,  respectively. The method was sensitive over the range from 10 ng/ml to 500 ng/ml of the tested  compounds.Results: The developed technique allows for determining valproic acid and its metabolites in a single sample; thus, the preliminary stage of separate sample preparation can be omitted, which increases the informative value of the assay without increasing its cost.Conclusion: This innovative methodology for the quantification of valproic acid and its metabolites in the blood plasma is expected to facilitate the individual approach to the treatment of patients with epilepsy, thereby increasing the efficacy and safety of the pharmacotherapy.

Simultaneous Determination of Phenolic Acids, Anthraquinones, and Flavonoids in the Aerial Part and the Fruit of Xanthium Sibiricum by LC- ESI- QTRAP-MS/MS

2019 ◽  
Vol 15 (5) ◽  
pp. 542-553
Author(s):  
Hui Zhao ◽  
Hao Cai ◽  
Juan-Xiu Liu ◽  
Sheng-Nan Wang ◽  
Xun-Hong Liu ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Phenolic Acids ◽  
High Performance ◽  
Aerial Part ◽  
Multiple Reaction Monitoring ◽  
Principal Component ◽  
Negative Ion ◽  
Xanthium Sibiricum ◽  
Relative Standard

Background: Xanthium sibiricum is a well-known traditional Chinese medicine (TCM) that has been commonly used to treat rhinitis and related nasal diseases. The aim of this study was to develop a comprehensive analytical method based on high-performance liquid chromatographyelectrospray ionization coupled with triple quadrupole-linear ion trap mass spectrometry (LC-ESIQTRAP- MS/MS) for the simultaneous determination of phenolic acids, anthraquinones, and flavonoids in the aerial part and fruit of Xanthium sibiricum. Methods: The separation was completed on Agilent ZORBAX SB-C18 column (250 × 4.6 mm, 5μm) using methanol and 0.2% (v/v) aqueous formic acid as the mobile phase. The target components were analyzed in negative ion mode with accurate and sensitive multiple reaction monitoring (MRM) mode. Results: The correlation coefficients of all the calibration curves were higher than 0.9994. Relative standard deviations of intra- and inter-day precisions of the eighteen components were all lower than 2.87% and the recoveries were in the range from 97.73% to 101.82%. The validated method was successfully applied to possess forty Xanthium sibiricum samples (Xanthii Herba, Xanthii Fructus, and processed Xanthii Fructus) collected from different places in P. R. China. Furthermore, principal component analysis (PCA) was performed to evaluate and classify the samples according to the contents of the eighteen bioactive components. Conclusion: All the results demonstrated that the developed method was useful and could be applied for the overall assessment of the quality of Xanthii Herba and Xanthii Fructus.

scholarly journals Studies of the pharmacokinetics of morroniside and loganin in rat after oral administration of raw and wine-processed Corni fructus by UPLC-QqQ-MS/MS

2022 ◽  
Vol 20 (2) ◽  
pp. 411-418
Author(s):  
Wei Wang ◽  
Xuechun Wang ◽  
Qiang Zhang ◽  
Ru Jia ◽  
Chunjie Du ◽  
...  
Keyword(s):  
Oral Administration ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Negative Ion ◽  
Pharmacokinetic Parameters ◽  
Tissue Samples ◽  
Multiple Reaction Monitoring Mode ◽  
The Mean ◽  
Corni Fructus ◽  
Negative Ion Mode

Purpose: To study the pharmacokinetics of morroniside (MR) and loganin (LG) in rats after oral administration of raw and wine-processed Corni fructus by UPLC-QqQ-MS/MS. Methods: Arctiin (AT) was used as internal standard, and the plasma or tissue samples were extracted twice using ethyl acetate. Electrospray ionization (ESI) negative ion mode was used, and the multiple reaction monitoring mode (MRM) was set in acquisition mode. The extraction and detection method is supported by selectivity, sensitivity, precision, accuracy, stability, extraction, recovery and matrix effect. The non-atrioventricular model of das2.0 software was used to calculate the pharmacokinetic parameters. Results: The absorption rate of MR (PTmax=0.092) and LG (PTmax=0.092) in Corni Fructus after wine-processing was faster in rats. The mean residence time was longer, and distribution of MR (PMRT0~t = 0.294) and LG (PMRT0~t = 0.000) in wine-processed Corni Fructus group increased in liver and kidneys. Conclusion: The proposed method has been successfully validated and is suitable for studying the pharmacokinetics of the two analytes in rats.

Rapid determination of patulin in medicinal hawthorn fruits by HPLC-MS/MS

2012 ◽  
Vol 5 (1) ◽  
pp. 31-36 ◽  
Author(s):  
L. Xiang ◽  
Y. Gao ◽  
D. Liu ◽  
M. Yang
Keyword(s):  
Rapid Determination ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Negative Ion ◽  
Liquid Liquid Extraction ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Hawthorn Fruit ◽  
Negative Ion Mode

An HPLC-tandem mass spectrometry method was developed for the determination of patulin (PAT) in dried medicinal hawthorn fruit, a well-known traditional medicine in China. Liquid-liquid extraction was applied in the sample preparation. Multiple reaction monitoring was performed at m/z 153/109 for PAT and m/z 317/273 for internal standard zearalenone in the negative ion mode with electrospray ionisation source. Good linearity was achieved when spiked PAT concentrations were in the range of 10-500 μg/kg, with coefficient being 0.9993. The limit of quantitation was 10 μg/kg. The extraction recoveries for the spiked PAT at concentrations of 20, 100 and 400 μg/kg were 64.5%, 64.6% and 63.9%, respectively, with relative standard deviations of 1.25%, 2.82% and 2.61%. The intra-day and inter-day precision were in the range of 2.2-9.6% and 5.9-6.4%. This rapid, sensitive and reliable method was applied in 25 batches of medicinal hawthorn fruit, in which PAT was detected in 8 batches, including those that were baked or charred.

1 An HPLC-MS/MS Method Using a Multitoxin Clean-up Column for Analysis of Seven Mycotoxins in Aquafeeds

2021 ◽  
Author(s):  
Siyuan Bi ◽  
Jingbing Xu ◽  
Xiaoshan Yang ◽  
Peng Zhang ◽  
Kaoqi Lian ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance ◽  
Correlation Coefficients ◽  
Negative Ion ◽  
Aflatoxin M1 ◽  
Contamination Level ◽  
Ionization Mass ◽  
External Standard Method ◽  
The Matrix ◽  
Negative Ion Mode

Abstract Background In Guangdong Province of China, the climate here is very wet, so there are many different fungus living in the aquatic feeds, which produce mycotoxins. These compounds contaminate agriculture products world-wide and represent a great threat to human health. It is necessary to determine their contamination level in aquatic feeds. Objective A high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) method was developed for the quantitative analysis of aflatoxin B1, aflatoxin M1, T-2 toxin, HT-2 toxin, deoxynivalenol, ochratoxin, and zearalenone in the fish and shrimp feed. Methods Samples were extracted with acetonitrile-water (V: V = 3:1), and degreased with acetonitrile-saturated hexane. Such obtained extract was cleaned up with a multitoxin column. The target compounds were separated on a C18 chromatographic column and analyzed simultaneously by electrospray ionization mass spectrometry in both positive or negative ion mode. Detected compounds were quantified by using the matrix-matched external standard method. Results Under the optimized conditions, good linearities for the analytes in corresponding concentration range were obtained with correlation coefficients (r2) higher than 0.9948. LOD ranged from 1.83 to 12.63 μg/kg, and LOQ ranged from 5.49 to 37.89 μg/kg. Average recoveries for the target mycotoxins at three spiked levels ranged from 80.5% to 116.5% with RSD ranging from 2.4% to 10.4%. 23 real aquafeed samples were determined by this method, and 7 kinds of toxins were all detected. Conclusions Obtained results showed that developed method could be successfully applied for the simultaneous determination of mycotoxins in aquatic feeds.

scholarly journals A QuEChERS-HPLC-MS/MS Method with Matrix Matching Calibration Strategy for Determination of Imidacloprid and Its Metabolites in Procambarus clarkii (Crayfish) Tissues

Molecules ◽  
2021 ◽  
Vol 26 (2) ◽  
pp. 274
Author(s):  
Qiuhong Yang ◽  
Xiaohui Ai ◽  
Jing Dong ◽  
Yongtao Liu ◽  
Shun Zhou ◽  
...  
Keyword(s):  
High Performance ◽  
Procambarus Clarkii ◽  
Rapid Determination ◽  
Multiple Reaction Monitoring ◽  
Negative Ion ◽  
Experimental Conditions ◽  
Neutral Alumina ◽  
Relative Standard ◽  
Primary Secondary Amine

We developed a method for determination of imidacloprid and its metabolites 5-hydroxy imidacloprid, olefin imidacloprid, imidacloprid urea and 6-chloronicotinic acid in Procambarus clarkii (crayfish) tissues using quick, easy, cheap, effective, rugged, and safe (QuEChERS) and high-performance liquid chromatography-triple quadrupole mass spectrometry. Samples (plasma, cephalothorax, hepatopancrea, gill, intestine, and muscle) were extracted with acetonitrile containing 0.1% acetic acid and cleaned up using a neutral alumina column containing a primary secondary amine. The prepared samples were separated using reverse phase chromatography and scanned in the positive and negative ion multiple reaction-monitoring modes. Under the optimum experimental conditions, spiked recoveries for these compounds in P. clarkii samples ranged from 80.6 to 112.7% with relative standard deviations of 4.2 to 12.6%. The limits of detection were 0.02–0.5 μg·L−1, the limits of quantification were 0.05–2.0 μg·L−1 and the method of quantification was 0.05–2.0 μg·kg−1. The method is rapid, simple, sensitive and suitable for rapid determination and analysis of imidacloprid and its metabolites in P. clarkii tissues.

Sign in / Sign up

Export Citation Format

Share Document