Simultaneous determination of ten constituents in herbal formulation Sipjeondaebo-tang using HPLC-PDA

A simple, rapid, and accurate high-performance liquid chromatographic method was applied to the quantitative determination of 10 components, namely, 5-hydroxymethyl-2-furaldehyde, albiflorin, paeoniflorin, liquiritin, ferulic acid, nodakenin, coumarin, cinnamic acid, cinnamaldehyde and glycyrrhizin in the traditional herbal formulation Sipjeondaebo-tang (SJDBT). All components were separated within 40 min using a Gemini C₁₈ column maintained at 40°C. The mobile phase was composed of 1.0% (v/v) aqueous acetic acid and 1.0% (v/v) acetic acid in acetonitrile by gradient elution. The flow rate was 1.0 mL/min and the detector was a photodiode array (PDA) set at 230, 254, 280, 320, and 330 nm. The calibration curves showed good linearity (r ² ≥ 0.9993) in different concentration ranges. The recovery of each component was in the range of 92.3–104.8%, with relative standard deviations (RSDs) less than 2.5%. The RSDs for intra- and inter-day precision were 0.09–2.8% and 0.07–3.2%, respectively. The amounts of the 10 components in SJDBT were in the range of 0.18–5.77 mg/g.     

Simultaneous Determination of Six Marker Compounds in Piper nigrum L. and Species Comparison Study Using High-Performance Thin-Layer Chromatography-Mass Spectrometry

JPC – Journal of Planar Chromatography – Modern TLC - The isolation and characterization of bioactive compounds from medicinal plants is usually a significant challenge in phytochemical...     

Simultaneous separation and determination of hydrocarbons and organochlorine compounds by using a two-step microcolumn.

The simultaneous separation and determination of a mixture of hydrocarbons and organochlorine compounds was successfully carried out by using sorption chromatography on a two-step microcolumn of silica and aluminium oxide for their fractionation, and a dual detector system. In addition to the separation and identification of hydrocarbons and heterocompounds containing nitrogen, oxygen and sulphur atoms, separation and identification of chlorinated hydrocarbons (dichlorobenzenes, p-chlorotoluene, hexachlorobutadiene, 1,2,4-trichlorobenzene and 2-chloronaphthalene), pesticides (chlorpicrin, aldrin, lindane, alpha- and beta-benzene hexachloride (BHC), endrin, dieldrin, endosulphan, methoxychlor) and herbicides (propanil, dichlobenil, trifluralin, difolatan) were achieved in mixtures containing polychlorinated biphenyl, strobane and chlordane.     

GC-EIMS analysis,antifungal and anti-aflatoxigenic activity of Capsicum chinense and Piper nigrum fruits and their bioactive compounds capsaicin and piperine upon Aspergillus parasiticus

Abstract

GC-EIMS analysis, antifungal- and anti-aflatoxigenic activities of the ethanolic extract of Capsicum chinense and Piper nigrum fruits and their main bioactive compounds were evaluated upon Aspergillus parasiticus. The GC-EIMS analysis showed capsaicin (50.49%) and piperine (95.94%) as the major constituents in C. chinense and P. nigrum, respectively. MIC₅₀ values revealed that capsaicin (39?μg/mL) and piperine (67?μg/mL) were lower than those from fruit extracts of C. chinense (381?μg/mL) and P. nigrum (68?μg/mL). Extracts and bioactive compounds showed anti-aflatoxigenic activity. Maximum aflatoxin inhibition occurred at 150?µg/mL of extracts and compounds. The present study showed satisfactory results concerning the effects of ethanolic extract of C. chinense and P. nigrum fruits upon A. parasiticus, showing the capabilities of inhibiting fungal growth development and altering aflatoxins production.     

New insecticidal amides from petroleum ether extract of dried Piper nigrum L. whole fruits

The petroleum ether extract of dried ground whole fruits of Piper nigrum L. afforded 20 compounds (1-20) including two new insecticidal amides named as pipnoohine (1), and pipyahyine (2), seven reported for the first time from this plant (12, 13, 15-17, 19, 20), and eleven known compounds (3-11, 14, 18). The structure of 1 has been elucidated as (2E,4E,12Z)-N-(4-methylpentyl)octadeca-2,4,12-trienamide and that of 2 as (2E,4E,11E)-12-(benzo[1,3]dioxol-5-yl)-N-(3-methylbutyl)dodeca-2,4,11-trien-amide through extensive ID-, 2D-NMR spectral studies and chemical reactions. The known compounds have been identified through comparison of their spectral data with those reported in literature. 1 and 2 exhibited toxicity at 35.0 and 30.0 ppm respectively against fourth instar larvae of Aedes aegypti L. by WHO method.     

HPLC法同时测定松果菊属中4种酚类化合物

松果菊属(Echinacea Moenck.)是原产于美洲的一类菊科野生花卉,也称“紫锥菊”。该属植物共有8种及数个变种,均为多年生草本,其中已开发为药品者主要为淡紫松果菊(E.palli-a)、狭叶松果菊(E.angustifolia)及紫花松果菊(E.purpurea)[1]。松果菊属植物主要用于促进机体的免疫功能     

Two New Insecticidal Amides and a New Alcoholic Amide from Piper nigrum Linn.

Three new amides, pipgulzarine ( 1 ), pipzorine ( 2 ), and piptahsine ( 3 ), have been isolated from the dried seeds of Piper nigrum Linn. along with nine known constituents: (2E,4E,8Z)‐N‐(isobutyl)eicosatrienamide, pellitorine, pipercide, piperine, stigmastanol, stigmasterol, decurrenal, stigmasterol 3‐O‐β‐D ‐glucopyranoside, and 5,10(15)‐cadinen‐4‐ol. The structures of the new constituents have been established as (2E,11E)‐12‐(benzo[1,3]dioxol‐5‐yl)‐N‐(2‐methylpropyl)dodeca‐2,11‐dienamide ( 1 ), (2E,12Z)‐N‐(4‐methylpentyl)octadeca‐2,12‐dienamide ( 2 ), and (2E,4S)‐4‐hydroxy‐N‐(2‐methylpropyl)hex‐2‐enamide ( 3 ). The structures of 1 – 3 were derived by spectral studies and chemical reactions, and by comparison of spectral data in the case of known constituents. Compounds 1 and 2 , and most of the already known compounds, exhibited toxicity against fourth instar larvae of Aedes aegypti Liston. The isolated (Z) double bond in 2 was assigned on the basis of its EI‐MS fragmentation pattern and its reaction with OsO₄. The (S) configuration at C(4) of 3 was determined by Horeau's method. This is the first report of the isolation of a 4‐methylpentylamide from P. nigrum, while shorter branched amides have been reported from this genus [1].     

Simultaneous estimation of hydroxychavicol and chlorogenic acid from Piper betel L. through RP-HPLC

A RP-HPLC method was developed (λ (max)?=?280) to quantify hydroxychavicol and chlorogenic acid in Piper betel Linn. The method was validated for linearity, limit of detection (LOD?=?3:1σ/S), limit of quantification (LOQ?=?10:1σ/S), precision, accuracy and ruggedness. The response was linear with good correlation between concentration and mean peak area through a coefficient of determinants (r (2)) of 0.9940, y?=?1.98e?+?004x?+?5.19e?+?004 and 0.9945, y?=?2.76e?+?004x?+?1.40e?+?005 with LOD 1.6?μg?mL(-1), 1.0?μg?mL(-1) and LOQ 5.0?μg?mL(-1) and 3.0?μg?mL(-1), respectively, for hydroxychavicol (28.56% w/w) and chlorogenic acid (0.40% w/w). The %RSD of precision and recovery of hydroxychavicol and chlorogenic acid were <2.0%. The proposed method was simple, accurate, specific, precise and reproducible.     

Simultaneous determination of butyltin and phenyltin species in sediments using ultrasound-assisted leaching

A fast and simple procedure is presented for the simultaneous leaching of butyl (mono, di and tributyl) and phenyl organotin species from sediment samples. Leached compounds are further ethylated with sodium tetraethylborate in aqueous medium, and analyzed by gas chromatography. After testing the stability of triphenyltin under different extraction conditions, ultrasound-assisted leaching at room temperature in the presence of acetic acid was been proposed as an extraction procedure compatible with the simultaneous determination of phenyl- and butyltin compounds in sediments. Recoveries between 70 and 90% were obtained for phenyl species in spiked samples prepared in the laboratory. Results for butyltin species were validated by use of the reference material PACS-2. Quantification limits, using GC-MIP-AES as measurement technique, were approximately 5-10 ng g(-1). Precision in the consecutive analysis of three sediment samples varied between 3 and 10%.     

Simultaneous determination of butyltin and phenyltin species in sediments using ultrasound-assisted leaching

A fast and simple procedure is presented for the simultaneous leaching of butyl (mono, di and tributyl) and phenyl organotin species from sediment samples. Leached compounds are further ethylated with sodium tetraethylborate in aqueous medium, and analyzed by gas chromatography. After testing the stability of triphenyltin under different extraction conditions, ultrasound-assisted leaching at room temperature in the presence of acetic acid was been proposed as an extraction procedure compatible with the simultaneous determination of phenyl- and butyltin compounds in sediments. Recoveries between 70 and 90% were obtained for phenyl species in spiked samples prepared in the laboratory. Results for butyltin species were validated by use of the reference material PACS-2. Quantification limits, using GC–MIP–AES as measurement technique, were approximately 5–10 ng g^–1. Precision in the consecutive analysis of three sediment samples varied between 3 and 10%. Received: 16 January 2001 / Revised: 12 March 2001 / Accepted: 13 April 2001     

SFE kinetics of bioactive compounds from Helianthus annuus L.

The kinetics of the supercritical fluid extraction of bioactive compounds from sunflower using CO₂ as solvent were studied in order to establish an efficient method for this extraction. The influence of time of extraction at different solvent flow rates was investigated. The extraction pressure and temperature were optimized in previous studies and these values used were 400 bar and 50°C. The extraction yields and the bioactivity levels of the extracts were also analysed. The results indicate that the most appropriate extraction time is between 120 and 180 min depending on the solvent flow and the pretreatment of the sample. The dried sample extracted at 40 g/min, the congealed sample extracted at the same flow and 180 min, and the dried sample extracted at 25 g/min for 120 min showed the best activity profiles. The extractions were carried out in a pilot plant with an extraction vessel with a capacity of 2 L.     

Simultaneous determination of organic ionic lead and mercury species using HPLC

A reversed-phase HPLC separation of organic ionic lead and mercury species has been achieved by using pre and on-column derivatisation with methyl thioglycolate. The separation parameters have been optimized and shown to permit a reproducible determination. For the enrichment of the compounds from water samples, the complexed organometallic species are concentrated on a precolumn. A recovery of 70 to 80% is achieved by using this one-line enrichment method.     

离子色谱-等离子体质谱联用测定热泉水样的砷形态

利用阴离子色谱与六极碰撞等离子体质谱联用的方法,在线同时测定水样的4种砷形态(As(Ⅴ),As(Ⅲ),MMA,DMA),并用于实际样品-热泉水中砷形态的测定.使用K2HPO4-KH2PO4为淋洗液等度淋洗,用Hamilton PRP-X100阴离子色谱柱分离,4种砷形态在7 min之内完全分离.调节淋洗液中K2HPO4与KH2PO4的比例可以优化峰的分离.地下水(含热泉水)基质、样品及淋洗液中的Cl-对砷形态的分离测定没有影响,淋洗液中的盐份在样品锥和截取锥上的积累对测定的影响很小.检出限分别为As(Ⅴ) 0.23 μg/L,As(Ⅲ) 0.30 μg/L,MMA 0.26 μg/L,DMA 0.54 μg/L.     

固相微萃取-气相色谱/质谱分析黑胡椒粉的挥发性成分

~~固相微萃取-气相色谱/质谱分析黑胡椒粉的挥发性成分@李祖光$浙江工业大学化学工程与材料学院!浙江杭州310014 @莫卫民$浙江工业大学化学工程与材料学院!浙江杭州310014 @胡伟$浙江工业大学化学工程与材料学院!浙江杭州310014 @乔剑峰$浙江工业大学化学工程与材料学院!浙江杭州310014固相微萃取;;气相色谱质谱法;;黑胡椒;;挥发性成分浙江省分析测试基金资助课题(02061).     

Simultaneous determination of seven compounds in snow lotus herb using high-performance liquid chromatography

A reversed-phase high-performance liquid chromatographic method is developed for the quantitative determination of seven components of Snow Lotus Herb (Saussurea tridactyla Sch.-Bip.ex Hook.f.): umbelliferonglucoside, luteolin-7-O-beta-D-glucoside, rutin, apigenin-7-O-beta-D-glucoside, kaempferol-3-O-beta-D-glucoside, apigenin-7-O-beta-D-rutinoside, and luteolin. Samples are analyzed by means of a reverse-phase column (Diamonsil C(18)) using methanol and water under gradient conditions as the mobile phase for 60 min. This method offers selectivity, accuracy, precision, linearity, and ruggedness, as well as efficiency and ease.     

Simultaneous determination of eight bioactive components of Cirsium setosum flavonoids in rat plasma using triple quadrupole LC/MS and its application to a pharmacokinetic study

Cirsium setosum (Willd.) MB. has been reported to exert significant anti‐hemorrhagic, anti‐inflammation, antimicrobial, sedative and detoxicating efficacy. It has been widely used to treat gastrointestinal bleeding, uterine bleeding, infectious hepatitis and cardiovascular disease in China. Recent studies have shown that flavonoids are the main active components in C. setosum. Nevertheless, to the best of our knowledge, there is no report concerning the simultaneous determinations and pharmacokinetics of constituents in C. setosum flavonoids in rat plasma. In this study, a rapid, sensitive and selective triple quadrupole liquid chromatography–mass spectrometry method was developed to determine eight analytes from the flavonoids of C. setosum in rat plasma. In addition, the pharmacokinetic study of the eight analytes in rats after oral administration of C. setosum flavonoids was successfully completed through this method. According to the pharmacokinetic parameters of the eight analytes, rutin, naringin, quercetin, acacetin, wogonin were the long‐acting components of the C. setosum flavonoids, with long elimination time and high bioavailability. Of note, the method developed in this study fills a blank in pharmacokinetic studies of C. setosum flavonoids. Our findings provide valuable views on the understanding of the absorption mechanism of C. setosum flavonoids and their clinical efficacy.     

Simultaneous determination of arsenic, selenium and antimony species using HPLC/ICP-MS

A new method for the simultaneous separation and determination of four arsenic species [As(III), As(V), monomethylarsonic acid and dimethylarsinic acid], three selenium species [Se(IV), Se(VI) and selenomethionine] as well as Sb(III) and Sb(V) is presented. The speciation was achieved by on-line coupling of anion exchange high-performance liquid chromatography (HPLC) with inductively coupled plasma mass spectrometry (ICP-MS). Chromatographic parameters such as the composition and pH of the mobile phase were optimised. Limits of detection are below 4.5 μg L^–1 (as element) for Sb(III) and the selenium species and below 0.5 μg L^–1 for the other species. Precisions of retention times were better than 2% RSD and of peak areas better than 8% RSD for all the species investigated. Received: 13 January 1999 / Accepted: 4 March 1999