scholarly journals Rapid Identification of two Species of Peucedanum by High-Performance Liquid Chromatography-Diode Array Detection-Electrospray Ionization Tandem Mass Spectrometry

2009 ◽  
Vol 4 (8) ◽  
pp. 1934578X0900400 ◽  
Author(s):  
Yanyan Tao ◽  
Jianguang Luo ◽  
Yuanyuan Lu ◽  
Deran Xu ◽  
Zhiguo Hou ◽  
...  

The fragmentation behaviors of the angular- and linear-type coumarins from Peucedanum praeruptorum Dunn and P. decursivum (Miq.) Maxim were simultaneously investigated by HPLC-DAD/ESI-MSn. For more structural identification, the fragment ions were analyzed and some possible fragmentation pathways were proposed. Different positions and numbers of the substituent also led to different fragment behaviors. Two types of coumarins from P. praeruptorum and P. decursivum were structurally elucidated by these techniques. In addition, UV spectra were applied to support the MS analysis. This is the first time that the two types of coumarins from herbal extracts have been differentiated by HPLC-DAD/ESI-MSn. The method further illustrated the importance of the ESI-MSn technique in the identification of different types of coumarins and was applied for the rapid differentiation of the two herbs.

2019 ◽  
pp. 135-147
Author(s):  
Daniil Nikolayevich Olennikov ◽  
Nina Igorevna Kashchenko

  Silene italica (L.) Pers. is a species of Caryophyllaceae family which introduced samples contain ecdysteroids that was previously shown (Meng et al., 2001). In this paper, the composition of ecdysteroids of wild-growing S. italica was shown. Using high performance chromatography with diode-array detection and electrospray ionization mass-spectrometry detection (HPLC-DAD-ESI-MS) twenty-two compounds assigned to the ecdysteroid group. The non-glycoside components of S. italica were included twelve compounds and integristerone A, 26-hydroxyintegristerone A, 22-deoxyintegristerone A, 2-deoxyintegristerone A, and 2-deoxypolypodine B were identified for the first time. Ten compounds were characterized as ecdysteroid monoglycosides containing hexose fragment as a carbohydrate part. Trer were derivatives of 20-hydroxyecdysone, polypodine B, ecdysone and 2-deoxypolypodine B. For the first time, the presence of 22-deoxyintegristerone A hexoside non-detected in plant objects was found. Comparative analysis of the ecdysteroids composition of S. italica and well studied species S. italica spp. nemoralis (Báthori et al., 2000, 2002, 2004; Pongrácz et al., 2003; Simon et al., 2002) indicates their proximity. Quantitative analysis of five ecdysteroid content in the organs of S. italica showed that they were unevenly distributed in the plant. The concentration of 20-hydroxyecdysone was 0.10–32.12 mg/g and the total ecdysteroids content was 0.10–40.92 mg/g of dry plant weight. In general, it should be noted that the ability to produce and accumulate ecdysteroids was also observed for the wild samples of S. italica, which cultural samples was noted as ecdysteroid concentrator.


Molecules ◽  
2018 ◽  
Vol 23 (11) ◽  
pp. 2869 ◽  
Author(s):  
Iván Taima-Mancera ◽  
Priscilla Rocío-Bautista ◽  
Jorge Pasán ◽  
Juan Ayala ◽  
Catalina Ruiz-Pérez ◽  
...  

Four metal-organic frameworks (MOFs), specifically UiO-66, UiO-66-NH2, UiO-66-NO2, and MIL-53(Al), were synthesized, characterized, and used as sorbents in a dispersive micro-solid phase extraction (D-µSPE) method for the determination of nine pollutants of different nature, including drugs, phenols, polycyclic aromatic hydrocarbons, and personal care products in environmental waters. The D-µSPE method, using these MOFs as sorbents and in combination with high-performance liquid chromatography (HPLC) and diode-array detection (DAD), was optimized. The optimization study pointed out to UiO-66-NO2 as the best MOF to use in the multi-component determination. Furthermore, the utilization of isoreticular MOFs based on UiO-66 with the same topology but different functional groups, and MIL-53(Al) to compare with, allowed us for the first time to evaluate the influence of such functionalization of the ligand with regards to the efficiency of the D-µSPE-HPLC-DAD method. Optimum conditions included: 20 mg of UiO-66-NO2 MOF in 20 mL of the aqueous sample, 3 min of agitation by vortex and 5 min of centrifugation, followed by the use of only 500 µL of acetonitrile as desorption solvent (once the MOF containing analytes was separated), 5 min of vortex and 5 min of centrifugation. The validation of the D-µSPE-HPLC-DAD method showed limits of detection down to 1.5 ng·L−1, average relative recoveries of 107% for a spiked level of 1.50 µg·L−1, and inter-day precision values with relative standard deviations lower than 14%, for the group of pollutants considered.


2010 ◽  
Vol 5 (5) ◽  
pp. 1934578X1000500
Author(s):  
Fengguo Xu ◽  
Ying Liu ◽  
Rui Song ◽  
Haijuan Dong ◽  
Zunjian Zhang

Da-Cheng-Qi decoction (DCQD) is a purgative prescription used in China and East Asia. To profile the constituents of this complex traditional Chinese medicine (TCM), a high-performance liquid chromatographic, electrospray ionization, tandem mass spectrometric (HPLC-ESI/MS/MS) analytical method was developed. After separation on a reversed-phase C18 analytical column using gradient elution, samples were analyzed by ESI-MS/MS in negative mode. As a result, a total of 37 compounds were detected, of which two tannins, three anthraquinones, two sennosides, five flavonoids and two lignans were unambiguously identified by comparison with standard compounds, and sixteen compounds were either tentatively identified or deduced according to their MS/MS data. The fragmentation pathways of many of the observed compounds, such as the tannins and lignans are reported for the first time. In addition, the identity of each peak in DCQD was explored by comparison with those of its three constituent herbs. The results indicated that tannins, anthraquinones and sennosides in DCQD originated from Radix et Rhizoma Rhei, flavonoids from Fructus Aurantii Immaturus, and lignans from Cortex Magnoliae officinalis. The present study provides an example of chemical constitution profiling in complex TCM systems using LC/MS/MS.


Molecules ◽  
2019 ◽  
Vol 24 (14) ◽  
pp. 2519 ◽  
Author(s):  
Yuri Mangueira Nascimento ◽  
Lucas Silva Abreu ◽  
Ramon Leal Lima ◽  
Vicente Carlos O. Costa ◽  
José Iranildo Miranda de Melo ◽  
...  

Zornia brasiliensis Vogel (Leguminosae) is a species popularly known in Brazil as “urinária”, “urinana”, and “carrapicho”, it is popularly used as a diuretic and in the treatment of venereal diseases. A specific methodology to obtain a saponin-enriched fraction and high-performance liquid chromatography coupled with diode array detection, ion trap mass spectrometry, and TOF-MS (HPLC-DAD-ESI-MS/MS) was applied for the analysis of triterpene saponins. The MS and MS/MS experiments were carried out by ionization in negative mode. Molecular mass and fragmentation data were used to support the structural characterization of the saponins. Based on retention times, high-resolution mass determination and fragmentation, 35 oleanane-triterpene saponins were tentatively identified in Z. brasiliensis.


2013 ◽  
Vol 8 (10) ◽  
pp. 1934578X1300801
Author(s):  
Kunming Qin ◽  
Hao Cai ◽  
Lijuan Zheng ◽  
Miao Zhang ◽  
Xinghai Zhang ◽  
...  

In this study, a simple, sensitive and reliable fingerprint analysis method by high-performance liquid chromatography coupled with diode array detection (HPLC-DAD) was developed for quality analysis of Bulbus Lilii, which is a famous traditional Chinese medicine and widely used as a restorative food. Then the developed method was subsequently applied to analyse 16 samples collected or purchased from different origins. Twelve common fingerprint peaks, including four definitely identified peaks, were found in total, and were involved for further characterisation and quality evaluation of Bulbus Lilii. The chemical quality of commercial samples collected from different origins varied obviously, indicating that more attention should be paid to the standardisation of the process of harvesting, manufacturing and storage of Bulbus Lilii. This is the first time that a new method has been established to control the quality of Bulbus Lilii through HPLC-DAD.


2020 ◽  
Vol 16 (4) ◽  
pp. 543-545 ◽  
Author(s):  
Imad Abdelhamid El Haci ◽  
Wissame Mazari ◽  
Fawzia Atik-Bekkara ◽  
Fatma Mouttas-Bendimerad ◽  
Fayçal Hassani

Background: Polygonum maritimum is one of the spontaneous halophyte plants of the Algerian coast. Many studies were carried out to evaluate the contents and the quality of phenolic compounds of this plant around the Mediterranean region. Objective: This paper intends to identify, for the first time, the phenolic compounds from the flower part of P. maritimum. Methods: RP-HPLC-PDA (Reversed Phase-High Performance Liquid Chromatography-Photo Diode Array) material was used for this purpose. Many standards were used and their retention times were stored in a local database. Identification was made on the basis of retention times of retained compounds and those found in the literature, and UV spectra of each peak. Results: This study intends to identify five phenolic acids (gallic, ferulic, sinapic, caffeic and syringic acids), one flavonol (rutin) and one flavanone (naringenin). Conclusion: P. maritimum is an important source of natural bioactive compounds that can be exploited for the benefit of many fields.


Marine Drugs ◽  
2020 ◽  
Vol 18 (10) ◽  
pp. 506
Author(s):  
Alfonso Prado-Cabrero ◽  
Ganjar Saefurahman ◽  
John M. Nolan

The harpacticoid copepod Tigriopus californicus has been recognized as a model organism for the study of marine pollutants. Furthermore, the nutritional profile of this copepod is of interest to the aquafeed industry. Part of this interest lies in the fact that Tigriopus produces astaxanthin, an essential carotenoid in salmonid aquaculture. Here, we study for the first time the stereochemistry of the astaxanthin produced by this copepod. We cultured T. californicus with different feeding sources and used chiral high-performance liquid chromatography with diode array detection (HPLC-DAD) to determine that T. californicus synthesizes pure 3S,3’S-astaxanthin. Using meso-zeaxanthin as feed, we found that the putative ketolase enzyme from T. californicus can work with β-rings with either 3R- or 3S-oriented hydroxyl groups. Despite this ability, experiments in the presence of hydroxylated and non-hydroxylated carotenoids suggest that T. californicus prefers to use the latter to produce 3S,3’S-astaxanthin. We suggest that the biochemical tools described in this work can be used to study the mechanistic aspects of the recently identified avian ketolase.


Author(s):  
Gorla S. Reddy ◽  
Chava V. N. Rao

Objective: Separation and identification of the process impurities in the manufacture of temsirolimus drug viz., rapamycin, temsirolimus regioisomer (monoester) (TS monoester), and temsirolimus diester (TS diester). Methods: During the process development of temsirolimus (TS), three process impurities-rapamycin, temsirolimus regioisomer (monoester) and temsirolimus diester-were detected by high-performance liquid chromatography (HPLC). Impurities were isolated by medium pressure liquid Chromatography (MPLC) and characterized by ESI-MS/MS, 1H NMR, FT-IR spectral data. Results: These impurities are characterised with the help of ESI MS/MS, 1H NMR, and FT-IR data. The impurities are identified and characterised as the process impurities. One of them is the starting material i.e. rapamycin and the other two are formed during the manufacture of the drug. This method offers advantages over using photodiode-array UV detection (LC-PDA) for the determination of peak purity, viz. components with similar UV spectra can be distinguished. Conclusion: The structures of these impurities were characterized as rapamycin, TS Monoester, and TS Diester. Out of these process impurities, rapamycin has been previously identified while the other two are previously unreported.


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