High-performance Liquid Chromatography Time-of-flight Mass Spectrometry Research Articles

The identification of key metabolites and mechanisms during isoniazid/rifampicin-induced neurotoxicity and hepatotoxicity in a mouse model by HPLC-TOF/MS-based untargeted urine metabolomics

The co-administration of isoniazid (INH) and rifampicin (RIF) is associated with hepatotoxicity and neurotoxicity. To systematically investigate the mechanisms of hepatotoxicity and neurotoxicity induced by INH/RIF, we used high performance liquid chromatography-time of flight mass spectrometry (HPLC-TOF/MS)-based untargeted metabolomics to analyze urine from a mouse model and screened a range of urinary biomarkers. Mice were orally co-administered with INH (120 mg/kg) and RIF (240 mg/kg) and urine samples were collected on days 0, 7, 14 and 21. Hepatotoxicity and neurotoxicity were assessed by samples of liver, brain and kidney tissue which were harvested for histological analysis. Toxicity analysis revealed that INH/RIF caused hepatotoxicity and neurotoxicity in a time-dependent manner; compared with day 0, the levels of 35, 82 and 86 urinary metabolites were significantly different on days 7, 14 and 21, respectively. Analysis showed that by day 21, exposure to INH+RIF had caused disruption in vitamin B6 metabolism; the biosynthesis of unsaturated fatty acids; tyrosine, taurine, hypotaurine metabolism; the synthesis of ubiquinone and other terpenoid-quinones; and the metabolism of tryptophan, nicotinate and nicotinamide. Nicotinic acid, nicotinuric acid and kynurenic acid were identified as sensitive urinary biomarkers that may be useful for the diagnosis and evaluation of toxicity.

A Multi-Approach Study of Phytochemicals and Their Effects on Oxidative Stress and Enzymatic Activity of Essential Oil and Crude Extracts of Rosmarinus officinalis

Rosmarinus officinalis or Rosemary is a highly valued medicinal vegetal, owing to its notable antispasmodic, anti-inflammatory, and antibacterial properties. In the current work, we aimed to identify the chemical components of the essential oil (EO) of R. officinalis and evaluate its biological properties using an in vitro approach. High performance liquid chromatography time-of-flight mass spectrometry (HPLC-TOF-MS) was utilized to analyze of the hydro-methanolic extract (HME), while gas chromatography–mass spectrometry (GC/MS) was considered during the analysis of the EO’s chemical composition. The antioxidant abilities of HME and the EO were assessed using diverse tests (DPPH, ABTS, GOR, CUPRAC, and FRAP). The anti-enzymatic properties were tested by the inhibition of cholinesterases, α-glucosidase, and tyrosinase enzyme. The HPLC-TOF-MS displayed the existence of flavonoids like luteolin glucuronide I and II, and a few known hydroxycinnamic acids. The EO contained three major components, namely, eucalyptol (28.7%), camphor (16.7%), and borneol (13.5%). The HME had a high total polyphenol content, as determined by the Folin–Ciocalteau method (335.37 ± 9.33 µg of gallic acid eq·mg−1). Notably, the analysis of the bioactivities of the HME and EO revealed comparatively that they possessed higher radical scavenging capacity in the DPPH, ABTS, and galvinoxyl assays, while EO exhibited a higher capacity for enzyme inhibition. Overall, our findings suggest that both the EO and HME extract of Algerian’s R. officinalis holds great usefulness in the pharmaceutical and nutraceutical fields due to its elevated polyphenol content and potent bioactivities.

Untargeted metabolomics analysis of omeprazole-enhanced chemosensitivity to cisplatin in mice with non-small cell lung cancer

Drug resistance of tumors remains a major barrier in cisplatin (CDDP)-based chemotherapy. Omeprazole (OME) is often utilized during chemotherapy to alleviate gastrointestinal symptoms. In a previous investigation, we demonstrated a protective effect of OME against CDDP-induced kidney injury. To further establish whether OME could enhance chemosensitivity to CDDP and the underlying mechanisms, an in vivo tumor-bearing mouse model with CDDP-resistant A549 non-small cell lung cancer (A549/CDDP) was established in the current study. A high-performance liquid chromatography-time of flight mass spectrometry (HPLC-TOF/MS)-based untargeted metabolomics approach for tumor tissue and serum was employed to explore the mechanisms underlying the enhanced therapeutic effects of co-administration of CDDP and OME. Notably, tumor weights of mice in the CDDP + OME group were significantly decreased compared with those treated with CDDP alone. HE and TUNEL staining revealed more significant apoptosis of tumor cells in the group co-administered CDDP + OME relative to CDDP alone. Overexpression of multidrug resistance-associated protein 2 in CDDP-resistant tumors was significantly reversed upon treatment with CDDP + OME. PCA score plots of the groups co-treated with CDDP + OME were clearly separated from those treated with CDDP alone in metabolomics analysis for tumor and serum samples, clearly suggesting that co-administration of OME enhances the antitumor effect of CDDP. Subsequently, 10 and 7 metabolites in CDDP + OME group with significant changes in tumor and serum compared with CDDP group, respectively, were identified. Pathway analysis both in tumor and serum samples revealed regulation of the metabolism of purines, several amino acids and riboflavin in enhanced chemotherapy with both OME and CDDP. The collective findings provide beneficial novel insights into drug-drug interactions, which could improve the application of CDDP in clinical practice.

A direct peptide reactivity assay using a high-throughput mass spectrometry screening platform for detection of skin sensitizers

Chemical-peptide conjugation is the molecular initiating event in skin sensitization. The OECD test guideline uses a high-performance liquid chromatography/ultraviolet (HPLC/UV) detection method to quantify chemical-peptide conjugation in a direct peptide reactivity assay (DPRA), which measures the depletion of two synthetic peptides containing lysine or cysteine residues. To improve assay throughput, sensitivity and accuracy, an automated 384-well plate-based RapidFire solid-phase extraction (SPE) system coupled with tandem mass spectrometry (MS/MS) DPRA was developed and validated in the presence of a newly designed internal standard. Compared to the HPLC/UV-based DPRA, the automated SPE-MS/MS-based DPRA improved throughput from 16 min to 10 s per sample, and substrate peptides usage was reduced from 100 mM to 5 μM. When implementing the SPE-MS/MS-based DPRA into a high-throughput platform, we found 10 compounds that depleted lysine peptide and 24 compounds that depleted cysteine peptide (including 7 unreported chemicals from 55 compounds we tested) in a concentration-response manner. The adduct formation between cysteine and cinnamic aldehyde and ethylene glycol dimethacrylate were further analyzed using high-performance liquid chromatography time-of-flight mass spectrometry (HPLC-TOF-MS) to confirm the conjugation. Overall, the automated SPE-MS/MS-based platform is an efficient, economic, and accurate way to detect skin sensitizers.

Sequential thermal dissolution of two low-rank coals and characterization of their structures by high-performance liquid chromatography/time-of-flight mass spectrometry and gas chromatography/mass spectrometry.

Gas chromatography/mass spectrometry (GC/MS) and high-performance liquid chromatography/time-of-flight mass spectrometry (HPLC/TOF-MS) were used to separate and reveal the molecular characteristics of organic matter in low-rank coals. Six soluble portions (SPs) were obtained by sequential thermal dissolution (TD) of two low-rank coals in the order of cyclohexane, acetone and methanol solvents at 300°C. Organic matter with different molecular characteristics were enriched in eachTD extract, which was further separated and analyzed by GC/MS and HPLC/TOF-MS using an electrospray ionization source in positive mode to obtain a comprehensive understanding of the structural composition of coals. Low polarity compounds like alkanes and arenes have a better solubility in cyclohexane. Phorone has the highest relative abundance in the acetone SPs, and the main compounds detected in the methanol SPs are alcohols and phenols. According to the data from HPLC/TOF-MS, most of the oxygen atoms are in the form of carbonyl and alkoxy groups. The nitrogen-containing compounds in SPs are mainly saturated aliphatic amines and pyridines. The sulfur-containing compounds mainly exist in the form of thioalkanes and thiophenes. Non-destructive methods were used to obtain soluble matter from coals, and different chromatographic and mass spectrometric techniques were used to separate and analyze the organic matter in coals. Detailed molecular structural information was obtained for the efficient and clean utilization of low-rank coals.

Analysis and fate of the hindered amine light stabilizer Tinuvin 622 in polyester powder coatings using high performance liquid chromatography / time of flight mass spectrometry

Hindered amine light stabilizers are used to protect polymers from heat- and light-induced degradation. In this study the oligomeric stabilizer Tinuvin 622 was analysed in-depth employing high performance liquid chromatography/time of flight mass spectrometry (HPLC/TOF-MS) to differentiate products of different manufacturers in respect of their terminating groups and oligomer length. Additionally, the behaviour of the stabilizer in uncured and cured polyester powder coatings was investigated regarding its interaction with the other coating components and chemical changes during the crosslinking process. The extraction efficiency was determined as a function of oligomer length and coating colour.

Water Extract of Cryphaea heteromalla (Hedw.) D. Mohr Bryophyte as a Natural Powerful Source of Biologically Active Compounds.

Bryophytes comprise of the mosses, liverworts, and hornworts. Cryphaea heteromalla, (Hedw.) D. Mohr, is a non-vascular lower plant belonging to mosses group. To the date, the most chemically characterized species belong to the liverworts, while only 3.2% and 8.8% of the species belonging to the mosses and hornworts, respectively, have been investigated. In this work, we present Folin–Ciocalteu and oxygen radical absorbance capacity (ORAC) data related to crude extracts of C. heteromalla obtained by three different extraction solvents: pure water (WT), methanol:water (80:20 v/v) (MET), and ethanol:water (80:20 v/v) (ETH). The water extract proved to be the best solvent showing the highest content of biophenols and the highest ORAC value. The C. heteromalla-WT extract was investigated by HPLC-TOF/MS (High Performance Liquid Chromatography-Time of Flight/Mass Spectrometry) allowing for the detection of 14 compounds, five of which were phenolic compounds, derivatives of benzoic, caffeic, and coumaric acids. Moreover, the C. heteromalla WT extract showed a protective effect against reactive oxygen species (ROS) generation induced by tert-butyl hydroperoxide (TBH) on the murine NIH-3T3 fibroblast cell line.

Transport of Potential Manure Hormone and Pharmaceutical Contaminants through Intact Soil Columns.

Although adding manure to agricultural soils is a commonly practiced disposal method and a means to enhance soil productivity, potential environmental contamination by any associated chemicals of emerging concern (CECs) such as hormones and pharmaceuticals is not well understood. Our objective was to provide field-relevant predictions of soil transport and attenuation of 19 potential manure CECs using undisturbed soil columns irrigated under unsaturated conditions. The CEC concentrations in leached water were monitored for 13 wk using high performance liquid chromatography-time of flight-mass spectrometry (HPLC-TOF-MS), after which time soil in the cores was removed and sampled for extractable CECs. Compounds quantified in column leachate included all four of the added sulfonamide antibiotics and the nonsteroidal, anti-inflammatory drug flunixin. Only trace amounts of several of the seven hormones, five remaining antibiotics, and two antimicrobials leached from the columns from exogenous soil additions. Soil residues of all 19 compounds were detected, with highest extractable amounts for 17α-hydroxyprogesterone > triclosan (antimicrobial) > flunixin > oxytetracycline. Those CECs with the highest recoveries as calculated by summing leached and extractable amounts were flunixin (14.5%), 17α-hydroxyprogesterone (5.3%), triclosan (4.6%), and sulfadimethoxine (4.8%). Manure management to prevent CEC contamination should consider the potential environmental problems caused by negatively charged compounds with the greatest mobility (flunixin and sulfadimethoxine) and those that have long residence times in soil (triclosan, 17α-hydroxyprogesterone, flunixin, and oxytetracycline). Flunixin is particularly important given its mobility and long residence time in soil.

Antiproliferative and Antioxidant Activities of Two Extracts of the Plant Species Euphorbia dendroides L.

Background: These days, the desire for naturally occurring antioxidants has significantly increased, especially for use in foodstuffs, cosmetics, and pharmaceutical products, to replace synthetic antioxidants that are regularly constrained due to their carcinogenicity. Methods: The study in hand aimed to appraise the antioxidant effect of two Euphorbia dendroides extracts using reducing power, anti-peroxidation, and DPPH (1,1 Diphenyl 2 Pycril Hydrazil) scavenging essays, in addition to the anticancer activity against two tumor cell lines, namely C6 (rat brain tumor)cells, and Hela (human uterus carcinoma)cell lines. Results: The results indicated that the ethyl acetate extract exhibited antiradical activity of 29.49%, higher than that of n-butanol extract (18.06%) at 100 µg/mL but much lower than that of gallic acid (78.21%).The ethyl acetate extract exhibits better reducing capacity and lipid peroxidation inhibitory activity compared to n-butanol extract but less than all tested standards. Moreover, the ethyl acetate extract was found to have an antiproliferative activity of more than 5-FU (5-fluoro-Uracil) against C6 cells at 250 µg/mL with IC50 and IC75 of 113.97, 119.49 µg/mL, respectively, and good cytotoxic activity against the Hela cell lines at the same concentration. The HPLC-TOF-MS (high performance liquid chromatography-Time-of-flight-Mass Spectrometry) analyses exposed the presence of various compounds, among which Gallic and Chlorogenic acids functioned as major compounds. Conclusions: The two extracts exhibited moderate anticancer abilities and behaved somewhat as average antioxidant agents. Based on the total phenolics and flavonoids contents, as well as HPLC results, it could be concluded that antiproliferative and antioxidant activities depend upon the content of different phenolics and flavonoids.

Effect of processing on the alkaloids in Aconitum tubers by HPLC-TOF/MS

According to the Chinese Pharmacopoeia 2015, only processed Aconitum tubers can be clinically applied, and the effect of processing is unclear. This research aimed to explore the effect of processing on cardiac efficacy of alkaloids in Aconitum tubers. First, the chemical ingredients in unprocessed and processed Aconitum tubers were identified and compared by using high performance liquid chromatography time-of-flight mass spectrometry (HPLC-TOF/MS) and multivariate pattern recognition methods. Then the representative alkaloids in Aconitum tubers, aconitine, benzoylaconine, and aconine, which belong to diester-diterpenoid alkaloids, monoester-diterpenoid alkaloids, and amine-diterpenoid alkaloids, respectively, were selected for further validation of attenuated mechanism. Subsequent pharmacological experiments with aconitine, benzoylaconine, and aconine in SD rats were used for validate the effect of processing on cardiac functions. After processing the Aconitum tubers, it was found that the contents of diester-diterpenoid alkaloids were reduced, and those of monoester-diterpenoid alkaloids and amine-diterpenoid alkaloids were increased, suggesting that diester-diterpenoid alkaloids were transformed into monoester-diterpenoid alkaloids and amine-diterpenoid alkaloids. Through further decocting the aconitine in boiling water, it was confirmed that the three alkaloids could be progressively transformed. Pharmacological experiments with aconitine, benzoylaconine, and aconine in SD rats showed that aconitine at a dose of 0.01mg/kg and aconine at a dose of 10mg/kg enhanced the cardiac function, while benzoylaconine at a dose of 2mg/kg weakened the cardiac function. The effect of processing is attributed to the transformation of the most toxic diester-diterpenoid alkaloids into less toxic monoester-diterpenoid alkaloids and amine-diterpenoid alkaloids.

The urinary metabolomic profile following the intake of meals supplemented with a cocoa extract in middle-aged obese subjects.

Metabolomics is used to assess the compliance and bioavailability of food components, as well as to evaluate the metabolic changes associated with food consumption. This study aimed to analyze the effect of consuming ready-to-eat meals containing a cocoa extract, within an energy restricted diet on urinary metabolomic changes. Fifty middle-aged volunteers [30.6 (2.3) kg m(-2)] participated in a 4-week randomised, parallel and double-blind study. Half consumed meals supplemented with 1.4 g of cocoa extract (645 mg polyphenols) while the remaining subjects received meals without cocoa supplementation. Ready-to-eat meals were included within a 15% energy restricted diet. Urine samples (24 h) were collected at baseline and after 4 weeks and were analyzed by high-performance-liquid chromatography-time-of-flight-mass-spectrometry (HPLC-TOF-MS) in negative and positive ionization modes followed by multivariate analysis. The relationship between urinary metabolites was evaluated by the Spearman correlation test. Interestingly, the principal component analysis discriminated among the baseline group, control group at the endpoint and cocoa group at the endpoint (p < 0.01), although in the positive ionization mode the baseline and control groups were not well distinguished. Metabolites were related to theobromine metabolism (3-methylxanthine and 3-methyluric acid), food processing (L-beta-aspartyl-L-phenylalanine), flavonoids (2,5,7,3',4'-pentahydroxyflavanone-5-O-glucoside and 7,4'-dimethoxy-6-C-methylflavanone), catecholamine (3-methoxy-4-hydroxyphenylglycol-sulphate) and endogenous metabolism (uridine monophosphate). These metabolites were present in higher (p < 0.001) amounts in the cocoa group. 3-Methylxanthine and l-beta-aspartyl-L-phenylalanine were confirmed with standards. Interestingly, 3-methoxy-4-hydroxyphenylglycol-sulphate was positively correlated with 3-methylxanthine (rho = 0.552; p < 0.001) and 7,4'-dimethoxy-6-C-methylflavanone (rho = 447; p = 0.002). In conclusion, the metabolomic approach supported the compliance of the volunteers with the intervention and suggested the bioavailability of cocoa compounds within the meals.

Effective degradation of tetracycline by mesoporous Bi2WO6 under visible light irradiation

Bi2WO6 was synthesized with a hydrothermal method at different pHs and used for the degradation of tetracycline (TC) in water. The mesoporous Bi2WO6 prepared at pH 1 (BWO-1) displayed the highest adsorption and degradation capacity to TC due to its large surface area and more efficient capacity to separate photogenerated electrons and holes. 97% of TC at 20 mg·L−1 was removed by BWO-1 at 0.5 g·L−1 after 120 min irradiation under simulated solar light. Only 31% of the total organic carbon (TOC) was removed after 360 min irradiation although the TC removal reached 100%, suggesting that TC was mainly transformed to intermediate products rather than completely mineralized. The intermediates were identified by high-performance liquid chromatography-time of flight-mass spectrometry (HPLC-TOF-MS) and possible photodegradation pathways were proposed.

Rapid identification of chemical constituents in Salvia chinensis by HPLC-TOF-MS

It's established a high-performance liquid chromatography-time of flight mass spectrometry(HPLC-TOF-MS) method to analyze chemical constituents in Salvia chinensis. The separation was performed on a SHISEIDO MG C18 reverse phase column (3.0 mm x 100 mm, 3 microm). The mobile phase consisted of acetonitrile (A) and water (containing 0.1% formic acid, B) was used as gradient elute. The gradient of a phase, 10%-90% (0-33 min), 90% (33-40 min). The flow rate was 0.6 mL x min(-1). Post-column split ratio was 2:1. Temperature of column was 25 degrees C. Time-of-flight mass spectrometer (TOF-MS) and electrospray ion source (ESI) was applied for qualitative analysis under positive ion mode, and mass scan range was m/z 100-1 000. As a result,28 of the major chemical constituents of S. chinensis were identified by HPLC-TOF-MS. In this study, a rapid and efficient method for studying the chemical constituents in S. chinensis by HPLC-TOF-MS was established, which paves a way for the quality control and further studies of the herb in vivo.

Development and Application of Chemical Analysis Methods for Investigation of Bio-Oils and Aqueous Phase from Hydrothermal Liquefaction of Biomass

Hydrothermal liquefaction (HTL) is an efficient second-generation technology for conversion of biomass or biomass waste products into bio-oils for e.g. the transport sector. The product consists of a bio-oil of varying viscosity and composition, as well as aqueous and gas-phase byproducts. In order to guide optimization of the HTL process with regard to conditions, catalysts, and feedstock, there is a need for standardized methods for product analysis. We have developed analytical methods to investigate the chemical composition of bio-oils produced in a continuous HTL plant using 11 different types of feedstocks and model compounds (sucrose, cellulose, sunflower oil, casein, gluten, cellulose mixed with protein, manures, sewage sludge, and Dried Distillers Grains with Solubles, DDGS). Bio-oils and aqueous phase byproducts were analyzed directly by gas-chromatography (GC) coupled with mass spectrometry (MS), while fatty acids (C10–C18) were specifically quantified using GC (with flame ionization detection) after derivatization into their methyl esters. In addition we developed and applied a new high-performance liquid chromatography time-of-flight mass spectrometry (HPLC-TOF-MS) method for detection of fatty acids (C14–C22) in the aqueous phase byproduct. Generally HTL bio-oils had a complex composition showing 100–200 separate peaks in the GC-MS chromatograms, but for most feedstocks, 30–50 peaks accounted for a large fraction of the total peak area. Grouping of identified products into chemical families provided a useful overview for characterization of the bio-oils. Fatty acids (C16 and C18) were major products from HTL of protein (gluten), sunflower oil, DDGS, sewage sludge, and some manure feedstocks, while other important compound groups in bio-oils included phenols, cyclopentenes, indoles, pyrroles, and amides. The aqueous phase contained products such as cyclopentenones, pyrazines, and fatty acids, also found in the bio-oils, which were probably present as micelles suspended in the aqueous phase.

Analysis of the chemical constituents of Hedan tablet by HPLC-TOF-MS method

Objective:To analyze the chemical constituents of Hedan tablet by high performance liquid chromatography-time of flight-mass spectrometry(HPLC-TOF-MS).Methods:The separation was performed on a Agilent Zorbax SB-Aq column(250 mm×4.6 mm,5 μm).The mobile phase consisting of acetonitrile(A)-1% acetic acid water solution(B) was used as gradient elute,0-50 min,0%-30%B,50-90 min,30%-75%B.The flow rate was 1 ml/min.TOF-MS was applied for qualitative analysis in positive ion mode with m/z of reference fragment 121.05 and 922.01.Results:The 33 chemical constituents of Hedan tablet were identified,and 5 groups of isomers were discriminated by TOF-MS and structure-relevant fragment ions.Conclusion:The HPLC-TOF-MS method is simple and reliable for analysis of the chemical constituents of Hedan tablets.

Qualitative analysis of the chemical constituents in Hedyotis diffusa by HPLC-TOF-MS

A high performance liquid chromatography–time-of-flight–mass spectrometry (HPLC-TOF-MS) method was developed for analysing the chemical constituents in Hedyotis diffusa, which is widely used as a traditional Chinese medicine (TCM) in the field of cancer treatment. The compounds were identified either by comparing the retention time and mass spectrometry data with those of reference compounds or by analysing mass spectrometry data and retrieving reference literature. Among the detected chromatographic peaks, nine components were unambiguously identified, most of which were iridoids. This study is expected to provide an effective and reliable pattern for comprehensive and systematic characterisation of the complex TCM systems.

Using cell membrane chromatography and HPLC-TOF/MS method for in vivo study of active components from roots of Aconitum carmichaeli

An offline two-dimensional system combining a rat cardiac muscle cell membrane chromatography time-of-flight mass spectrometry (CMC-TOF/MS) with a high Performance liquid chromatography time-of-flight mass spectrometry (HPLC-TOF/MS) was established for investigating the parent components and metabolites in rat urine samples after administration of the roots of Aconitum carmichaeli. On the basis ofthe analysis of the first dimension, retention components of the urine sample were collected into 30 fractions (one fraction per minute). Then offline analysis of the second dimension was carried out. 34 compounds including 24 parent alkaloids and 10 potential metabolites were identified from the dosed rat urine, and then binding affinities of different compounds on cell membranes were compared and influences of some functional groups on activity were estimated with the semi-quantification and curve fitting method. As a result, binding affinities decreased along with the process of deacylation, debenzoylation and demethylation, which may be related to the alleviation of toxicity in the procedure of herb processing or metabolism. Moreover, some minor components in rat urine (Songorine, 14-benzoylneoline, Deoxyaconitine, etc.) exerted relatively strong affinity on cell membranes are worth exploring. The results delivered by the System suggest that the CMC can be applied to in vivo study.

Acute interstitial nephritis due to administration of multiple antibiotics:a case report

Objective:To identify the chemical components in traditional Chinese herbal medicine Ginseng by high performance liquid chromatography diode array detector (HPLC-DAD) and High performance liquid chromatography-time of flight mass spectrometry (HPLC-TOF/MS).Methods: An Agilent Zorbax XDB-Cl8 column (250 mm×4.6 mm,5 μm) was used for isolation and identification of chemical components in Ginseng with a mobile phase of acetonitrile and water in gradient elution.A gradient program was used as follows:1-35 min,19% A; 35-55 min,19%-29% A; 55-70 min,29% A; 70-110 min,29%-40% A; 110-150 min,95% A.The flow rate was set at 1.0 ml/min,the injection volume was 20 μl,and the column temperature was set at 20℃.The time-of-flight mass spectrometer was equipped with an EIS ion source.Scanning mass range was between m/z 100-1 350.Results: Thirty-nine chemical compounds in Ginseng were identified unequivocally.Conclusion: Chromatographic demonstration of 39 chemical compounds of Ginseng in one run is achieved by HPLC-TOF/MS,which provides a foundation for further study on the metabolism and action mechanism of traditional Chinese herbal medicine.

HPLC-TOFMS in rapid separation and identification of chemical components in &lt;I&gt;Oldenlandia diffusa&lt;/I&gt; and its injection preparations

Objective To rapidly separate and identify the chemical components in traditional Chinese herbal medicine of Oldenlandia diffusa and its injection preparations by high performance liquid chromatography-time of flight mass spectrometry(HPLC-TOFMS).Methods An Agilent Zorbax XDB-Cl8 column(250 mm×4.6 mm,5 μm) was used for separation and identification of chemical components in Oldenlandia diffusa,with a mobile phase of 0.3% acetic acid(A) and methanol(B) in gradient elution,0-30 min,30%-90%B.The flow rate was set at 1.0 ml/min and the injection volume was 10 μl.The time-of-flight mass spectrometer was equipped with an EIS ion source.The scanning mass range was between m/z 100-1 000.Results The traditional Chinese medicine of Oldenlandia diffusa and its injection preparation were on-line separated and characterized by HPLC-TOFMS,and 11 chemical compounds were identified in Oldenlandia diffusa,6 compounds in market injection preparation,and 2 compounds in the injection prepared by ourselves.Conclusion Chromatographic demonstration of chemical compounds in Oldenlandia diffusa in one run provides a foundation for the further studying the metabolism and mechanism of Oldenlandia diffusa and its injection preparations.

Analysis of synthetic antioxidants and preservatives in edible vegetable oil by HPLC/TOF-MS

The application of high performance liquid chromatography time-of-flight mass spectrometry (HPLC/TOF-MS) for the qualitation and quantitation of 11 synthetic antioxidants and preservatives in edible vegetable oil samples is reported here. The qualitation by HPLC/TOF-MS is accomplished with the accurate mass of the deprotonated molecules [M−H] −, along with the accurate mass of their main fragment ion. In order to obtain sufficient sensitivity for quantitation purposes (using deprotonated molecule), segment programme of fragmentor voltage is designed in negative ion mode. The mass accuracy typically obtained is routinely better than 5 ppm. The 11 compounds behave linearly in the 0.05–5.0 mg/kg concentration range, with correlation coefficient >0.997. The recoveries at the tested concentrations of 0.1–2.0 mg/kg are 65.8–106.9%, with coefficients of variation <8.1%. The method illustrated is suitable for routine qualitative and quantitative analyses of synthetic antioxidants and preservatives in edible vegetable oils.