Determination of triptolide and triptonide in human plasma by high-performance liquid chromatography

An isocratic high-performance liquid chromatographic method for determination of triptolide and triptonide in human plasma is described. Plasma samples were extracted with OasisHLB solid-phase extraction (SPE) cartridges. After pretreatment, they were separated on a SymmetryShieldRP(18) column with a mobile phase of acetonitrile-water (40:60,v/v) at 40 degrees C. The effluent was monitored at UV 217 nm. Linearity (0.010-1.0 mg/L) was good, and the lower limit of detection was 3 ng/mL for triptolide and 4.5 ng/mL for triptonide (S/N = 3). The relative standard deviations of intra- and inter-day assay were less than 15% and the recoveries were better than 80%. The developed method was applied to the determination of triptolide and triptonide concentration in a patient's plasma after taking the medicament containing Tripterygium wilfordii Hook. F.     

THE CRYSTAL AND MOLECULAR STRUCTURE OF TRIPTONIDE

<正> Triptonide, C20H22O6, was extracted from tripterygium wilfordii Hook F. of Fujian province and its structure was determined by X-ray crystallo-graphic analysis, Mr = 358. 39, monoclinic, P21,a = 11. 144(5), 6 = 6. 467(2), c= 12. 681(6)(?), β=103.54(4)°, V= 888. 4(?)3. Z = 2, F(000) = 380, Dc= 1. 34g/ cm3. The structure was solved by direct methods and refined by full matrix least-squares method to a final R value of 0. 042 for 1934 reflections with I> 3σ(I). Crystals of triptonide are isostructural with those of triptolide.     

Studies on the Chemical Constituents and Bioactivities of Tripterygium Wilfordii

Tripterygium wilfordii Hook (TW) is a medicinal plant distributed widely in southern china. This plant was recently found to possess anti-inflammatory, antitumor and immunosuppressive activities. Some preparation of the plant root has been used for the treatment of rheumatoid arthritis, systemic acne rosacea, nephritis and some skin diseases. Chemical studies on this plant and its preparation have shown they contain a large number of sesquiterpenoid, diterpenoids, triterpenoids and alkaloids in which some diterpene triepoxy lactones such as triptolide and triptonide etc are considered as mainly active compounds.     

Spectrophotometric determination of uranium(VI) using a synergic mixture of ethyl acetoacetate and pyridine

A method is proposed for the extractive spectrophotometric determination of uranium(VI) using the synergic combination of ethyl acetoacetate (EAA) and pyridine (Py) as extractants. The optimum conditions have been evaluated by varying pH and ethyl acetoacetate and pyridine concentration. The nature of the extracted species has been determined by 1g D-1g C plots and the extracted species was found to be UO₂(EAA)₂.Py. The method has been applied for the separation and determination of uranium(VI) from synthetic mixtures.     

Substoichiometric determination of cobalt in crud

A substoichiometric extraction method with nitroso-R salt (NRS) has been studied for the determination of trace Co in crud. The Co-NRS complex is extracted substoichiometrically into Capriquat-CHCl3 at pH 6.5-9.0 in 20 min of shaking time. The analytical results obtained by the method are within 3% of relative error in the determination range of 5 to 50 micrograms. The proposed method is simple and has sensitivity of 0.5 micrograms, though Fe(II), Ni(II) and Cu(II) seriously interfere. The results applied for the determination of trace Co in crud are described.     

Flow rate gradient high-speed counter-current chromatography separation of five diterpenoids from Triperygium wilfordii and scale-up

In this paper, high-speed counter-current chromatography (HSCCC) instruments with different gravitational forces were applied for the separation of bioactive compounds from Triperygium wilfordii Hook.f. The critical parameters including sample concentration, sample volume and flow rate were first optimized on an analytical Mini-DE HSCCC system, and then scaled up to a preparative TBE 300A HSCCC system. Although this scale-up process was performed using different CCC instruments with different centrifuges and gravitational forces, the same resolutions were obtained and the elution time could be predictable. Five diterpenoid compounds and one unknown compound were separated from Triperygium wilfordii Hook.f. by HSCCC with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (HEMW) (3:2:3:2, v/v/v/v). This one-step flow gradient separation produced triptonide (25 mg), isoneotriptophenolide (77 mg), hypolide (83 mg), unknown compound (1 mg), triptophenolide (42 mg), triptonoterpene methyl ether VI (37 mg) from 320 mg crude extract with purities of 98.2%, 96.6%, 98.1%, 95.3%, 95.1%, and 96.5%, respectively. Their purities and structures were identified by high-performance liquid chromatography, mass spectrometry and NMR. This paper demonstrates that analytical CCC plays an important role in optimizing parameters and scale-up process when analytical CCC and preparative CCC are supplied by different manufacturers with different gravitational forces, and the scale-up process from analytical CCC to preparative CCC is still predictable.     

Determination of tin by resin-suspension electrothermal atomic absorption spectrometry after enrichment as the complex with ammonium pyrrolidinedithiocarbamate.

A resin-phase extraction method has been optimized for the trace determination of tin(II) by ETAAS. Tin(II) was extracted on a finely divided anion exchange resin as the complex with ammonium pyrrolidinedithiocarbamate (APDC). The resin was collected on a membrane filter and then dispersed in 1.00 ml of 1 mol l(-1) nitric acid containing 100 microg of Pd(II) and 60 microg of Ni(II). The resulting resin suspension was subjected to GFAAS. The proposed method was applied to the determination of tin(II) in hydrochloric acid.     

高效液相色谱梯度法测定雷公藤制剂中雷公藤甲素的含量

采用高效液相色谱梯度法分离测定雷公藤制剂中雷公藤甲素的含量,用国产YWG色谱柱分离,二极管阵列检测器检测,所得三维光谱与空白光谱进行差减,取波长218nm处色谱图积分,定量。与等度法比较,梯度法具有更高的分离度、灵敏度,测定雷公藤口服液中雷公藤甲素的质量浓度为202．0μg／L,每片雷公藤片剂含甲素11．74μg,结果显著低于等度法和标示量（P<0．05）。     

Determination of trace phosphate ion with 3,3',5,5'-tetramethylbenzidine using a flotation-extraction preconcentration method and spectrophotometric detection

A flotation-extraction method for sensitivity enhancement in spectrophotometry is proposed. The method is based on the reaction among molybdate, phosphate and 3,3',5,5'-tetramethylbenzidine (TMB) in acidic medium to form an color charge transfer complex ion. It forms an ion associate with positive ions and floated at the water/benzene interface simultaneously, and then extracted by the DMSO-formic acid directly and determined by spectrophotometry. The proposed method is simple and convenient. The apparent molar absorptivity is 4.03x10(5) L mol(-1) cm(-1) at 458 nm. The proposed method has been applied to the determination of phosphate in wastewater with satisfactory results.     

Rapid quantification of cyanamide by ultra-high-pressure liquid chromatography in fertilizer,soil or plant samples

A rapid and simple method for determination of cyanamide in fertilizer, soil and plants has been developed. In this method, cyanamide is extracted with 2% acetic acid and the extract separated by centrifugation. It is then purified by passing through a membrane filter. The extract was derivatized with 6-aminoquinolyl-N-hydroxysuccinimidyl-carbamate and the derivatized compound separated by ultra-high-pressure liquid chromatography. It is then detected with a UV detector at 260 nm by the same method as is used for amino acid analysis. The proposed method is fast, simple and cheap and also has good selectivity and sensitivity for the determination of cyanamide in a wide range of biotic and abiotic materials.     

萃取分光光度法测定盐酸洛美沙星

提出了测定盐酸洛美沙星 (LMX)的萃取分光光度法 ,该法基于在弱酸性条件下 ,盐酸洛美沙星与溴甲酚绿 (BMG)反应生成可被三氯甲烷萃取的离子对缔合物 ,其最大吸收波长为 415nm。药物浓度在 1～ 15mg/L(r=0 .9997)范围内符合比耳定律。表观摩尔吸收系数ε =2 .5× 10 4 L·mol-1·cm-1。最低检出限为 0 .0 14mg/L。回收率为 98.9%～ 10 1.6 %。该法可成功的用于药物制剂中洛美沙星含量的测定     

Extractive fluorimetric determination of ultratraces of lead with 18-crown-6 and eosin

A highly sensitive and selective spectrofluorimetric procedure for the determination of lead in the range 0.003-0.5 ppm, based on solvent extraction of the ion-pair formed between the eosinate anion and the cationic complex of Pb(2+) with 18-crown-6, has been developed. The relative standard deviation is 3.7% at the 0.1 ppm level. The metal :ligand: counter-ion molecular ratio in the ion-pair extracted is 1:1:1, but aggregation of the complex may occur in the organic phase. The system proposed is exceptionally selective for extraction of lead in the presence of other cations frequently associated with it. The proposed method has been tested in the determination of lead in tap water. The results show good agreement with those found by the more common extractive atomic-absorption method using ammonium tetramethylenedithiocarbamate.     

连续小波变换-独立成分回归算法及其在多组分分析中的应用

采用连续小波变换（CWT）对光谱数据进行处理，用独立成分分析（ICA）进行特征提取，再用回归分析方法对被测组分进行测定，建立了连续小波变换一独立成分回归（CWT-ICR）方法。方法用于肉样品中水分、脂肪和蛋白质多组分的同时测定，所得结果与化学法测得结果相符。     

Complexometric titration of calcium in the presence of larger amounts of magnesium

A simple and accurate titrimetric determination of calcium in the presence of larger amounts of magnesium is proposed. Calcium is extracted into a small volume of organic solvent as its glyoxal-bis(2-hydroxyanil) complex, and the calcium is titrated with EGTA. The end-point is sharp, and occurs when the red colour of the organic layer vanishes. This method has been successfully applied to the determination of calcium in sea-water with an error less than 0.1%.     

Shortened screening method for phosphorus fractionation in sediments: A complementary approach to the standards, measurements and testing harmonised protocol

The SMT protocol, a sediment phosphorus fractionation method harmonised and validated in the frame of the standards, measurements and testing (SMT) programme (European Commission), establishes five fractions of phosphorus according to their extractability. The determination of phosphate extracted is carried out spectrophotometrically. This protocol has been applied to 11 sediments of different origin and characteristics and the phosphorus extracted in each fraction was determined not only by UV-Vis spectrophotometry, but also by inductively coupled plasma-atomic emission spectrometry. The use of these two determination techniques allowed the differentiation between phosphorus that was present in the extracts as soluble reactive phosphorus and as total phosphorus. From the comparison of data obtained with both determination techniques a shortened screening method, for a quick evaluation of the magnitude and importance of the fractions given by the SMT protocol, is proposed and validated using two certified reference materials.     

Simultaneous spectrophotometric determination of fat-soluble vitamins in multivitamin pharmaceutical preparations

A spectrophotometric method is proposed for the simultaneous determination of vitamins A, D and E in multivitamin pharmaceutical preparations. This is based on multiple linear regression. Most vitamins are directly extracted from the preparations into n-hexane. Microen-capsulated vitamin A preparations require pretreatment of de-encapsulation before the vitamin is extracted. The wavelength range to be used for each preparation and the optimum spectral mode (absorbance or first-derivative) has been chosen in order to assure correct quantitation and avoid interferences from other absorbing species also extracted by n-hexane. The results obtained were validated by simultaneous HPLC analyses for accuracy and precision.     

Automatic determination of total aliphatic amines by on-line photometric liquid-liquid microextraction

An automatic flow method for the determination of total aliphatic amines has been developed. Using an integrated micro extraction unit at the detection point that allows continuous on-line monitoring of small organic plug from which amines are extracted. It is based on the formation of ion-pairs between aliphatic amines and sodium 1,2-naphthoquinone-5-sulphonate that are subsequently extracted into chloroform. The gradual enrichment of the organic phase with the ion-pair is continuously monitored at 460 nm. Absorbance readings at a fixed time and the slopes of absorbance-time recordings are the measured parameters used for determination purposes. The proposed method has been applied to the determination of total aliphatic amines in both synthetic and real (food) samples.     

Determination of Ketotifen Fumarate in Raw Material and Pharmaceutical Products Using Ion‐pair Formation

Abstract

A simple and sensitive extractive spectrophotometric method has been described for the determination of Ketotifen. The developed method is based on the formation of a colored ion‐pair complex (1∶1 drug/dye) of Ketotifen and bromocresol green in buffer pH 3 and extraction in chloroform. The extracted complex shows absorbance maxima at 423 nm. Beer's law is obeyed in the concentration range of 5.15–61.91 µg/ml. The proposed method has been applied successfully for the determination of drug in commercial tablets and syrup dosage form. No significant interference was observed from the excipients commonly used as pharmaceutical aids with the assay procedure.     

Extraction and spectrophotometric determination of cobalt(II) with isonitroso-5-methyl-2-hexanone

A simple and selective method is proposed for the extraction of cobalt(II) for its spectrophotometric determination using (HIMH) as an extractant. Cobalt(II) forms a yellow coloured complex with HIMH which can be extracted into chloroform. The calibration curve is rectilinear in the concentration range 0.1–5.0 μg ml⁻¹ of cobalt(II). The extracted species shows an absorption maximum at 400 nm with molar absorptivity of 1.135×10⁴ l mol⁻¹ cm⁻¹. The method has been applied for the determination of cobalt in synthetic mixtures, pharmaceutical, biological and high speed steel samples.     

Pyraflufen-ethyl residues in soil by solid phase extraction and high-performance liquid chromatography with UV detection.

Solid-phase extraction (SPE) procedure for cleanup followed by HPLC-UV method has been investigated for the determination of pyraflufen-ethyl residues in soil. The pesticide is extracted from the sample with acetone-water (80:20, v/v) and the extract is loaded onto an octadecyl (C(18)) column. The pesticide is eluted with acetonitrile and determined by HPLC with a UV detector. Using an acetone-water extraction followed by a C(18) cleanup, this method is characterized by recovery >90.1%, precision <5.8% RSD and sensitivity of 0.01 mg/kg. The proposed method has been successfully employed for the determination of the degradation dynamics of pyraflufen-ethyl in four agricultural soil samples under laboratory conditions.