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  • Author or Editor: S.-Q. Liu x
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Abstract  

The thermal decomposition behaviour of the complexes of rare earth metals with histidine: RE(His)(NO3)3 H2O (RE=La—Nd, Sm—Lu and Y; His=histidine) was investigated by means of TG-DTG techniques. The results indicated that the thermal decomposition processes of the complexes can be divided into three steps. The first step is the loss of crystal water molecules or part of the histidine molecules from the complexes. The second step is the formation of alkaline salts or mixtures of nitrates with alkaline salts after the histidine has been completely lost from the complexes. The third step is the formation of oxides or mixtures of oxides with alkaline salts. The results relating to the three steps indicate that the stabilities of the complexes increase from La to Lu.

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Summary

A simple hydrolysis method has been developed for determination of phenylethanoid glycosides in Lamiophlomis rotata (L.R.). Different kinds of phenylethanoid glycosides were hydrolyzed in hydrochloric acid solution to produce corresponding phenethyl alcohols and cinnamic acids, mainly containing hydroxytyrosol, homovanillyl alcohol, 3,4-dimethoxyphenethyl alcohol, caffeic acid, fumalic acid and 3,4-dimethoxycinnamic acid. The six analytes could be determined simultaneously by high-performance liquid chromatography (HPLC). The effects of mobile phase, pH and concentration of running buffer, detection wavelength, flow rate and injection volume were also investigated. Under the optimum conditions, the six hydrolyzates could be perfectly separated within 45 min. The response was linear over four orders of magnitude with detection limits (S/N = 3) ranging from 1 × 10−8 to 1.5 × 10−4 mol L−1 for the analytes. The method has been successfully applied to the analysis of real sample Du-Yi-Wei capsule and Qi-Zheng-Yan-Tong patch, with satisfactory results.

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Abstract  

Excess molar enthalpies of binary mixtures for tributyl phosphate (TBP)+methanol/ethanol were measured with a TAM air Isothermal calorimeter at 298.15 K and ambient. The results for xTBP+(1–x)CH3OH are negative in the whole range of composition, while the values for xTBP+(1–x)C2H5OH change from positive values at low x to small negative values at high x. The experimental results have been correlated with the Redlich–Kister polynomial. IR spectra of the mixtures were measured to investigate the effect of hydrogen bonding in the mixture.

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Abstract  

The eight solid complexes of zinc with L--methionine or L--histidine were prepared. The thermal decomposition processes of these complexes were determined by means of TG-DTG. The results show that their decomposition processes can be divided into three steps except for the complex Zn(Met)2 the decomposition of which is completed in one step. All the final products are ZnO.

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Abstract  

The enthalpies of solution in water of RE(His)(NO3)3 H2O (RE=La—Nd, Sm—Lu, Y) were measured calorimetrically at 298.15 K, and the standard enthalpies of formation of RE(His)aq 3+ (RE=La—Nd, Sm—Lu, Y) were calculated. The plot of the enthalpies of solution vs. the atomic numbers of the elements in the lanthanide series exhibits the tetrad effect.

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Summary

A simple and rapid HPLC method using a photodiode array (PDA) detector for the analysis of 3-hydroxycarboplatin and its related complex has been established for the first time. Separation of 3-hydroxycarboplatin and 3-hydroxy-1,1-cyclobutanedicarboxylic acid (3-HO-cbdca) was carried out on a Phenomenex ODS3 column using an aqueous solution containing 50 mM ammonium acetate and 5 mM sodium 1-octanesulfonate as the mobile phase. The flow rate was 0.8 mL min−1, the column temperature was 40°C, and the detection wavelength was 230 nm for 3-hydroxycarboplatin and 220 nm for 3-HO-cbdca. Different analytical performance parameters such as precision, accuracy, linearity, stability of the solution, specificity, limit of detection (LOD), limit of quantification (LOQ), and system suitability were determined using the Empower 2 software. The calibration curve of standard 3-hydroxycarboplatin showed good linearity (r = 0.9995) within the range 0.5–1.4 mg mL−1. The method was accurate and precise, with an average accuracy of 100.4% (RSD = 1.53%, n = 9), and the results of the system suitability test showed symmetrical peaks, good resolution (R s), and repeatability. It can be applied to the quality control of 3-hydroxycarboplatin.

Open access

Shuganjieyu (SGJY) capsule is a classical formula widely used in Chinese clinical application. In this paper, an ultra-performance liquid chromatography coupled with electrospray ionization and ion trap mass spectrometry has been established to separate and identify the chemical constituents of SGJY and the multiple constituents of SGJY in rats. The chromatographic separation was performed on a C18 RRHD column (150 × 2.1 mm, 1.8 μm), while 0.1% formic acid–water and 0.1% formic acid–acetonitrile was used as mobile phase. Mass spectral data were acquired in both positive and negative modes. On the basis of the characteristic retention time (R t) and mass spectral data with those of reference standards and relevant references, 73 constituents from the SGJY and 15 ingredients including 10 original constituents and 5 metabolites from the rat plasma after oral administration of SGJY were identified or tentatively characterized. This study provided helpful chemical information for further pharmacology and active mechanism research on SGJY.

Open access

Abstract  

The iron contents in the hair and blood samples of 37 juvenile athletes who were supplemented with 0, 8 and 16 mg Fe/day, respectively, in the food of ferrous gluconatecontaining chocolate for 3 months were determined before and after the supplementation by INAA, SRXRF and blood analysis. The experimental results showed that after supplementation of the iron-fortified food, the normal ferritin level in the blood of the male athletes was attained and the iron content in the hair was increased with supplementation, but both are not in the positive proportion. Most of the female athletes had similar results. It is suggested that supplementation of 8 mg iron/day to juvenile athletes may be desirable.

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Compound danshen preparations (CDPs) are used clinically for the treatment of cardiovascular and cerebrovascular diseases. By using the quantitative analysis of multi-components by single-marker (QAMS) method, sixteen compounds (danshensu, protocatechuic acid, protocatechuicaldehyde, caffeic acid, rosmarinic acid, lithospermic acid, notoginsenoside R1, salvianolic acid B, ginsenoside Rg1, ginsenoside Re, salvianolic acid A, salvianolic acid C, ginsenoside Rb1, ginsenoside Rd, cryptotanshinone, and tanshinone IIA were quantified on an ACQUITY ultraperformance liquid chromatography (UPLC) HSS T3 column (2.1 × 100 mm, 1.8 μm) with the mobile phase consisting of 0.1% formic acid aqueous solution (A) and acetonitrile (B) using a gradient elution at the flow rate of 0.30 mL/min in 30 min at 30°C, which was also validated by UPLC-diode array detection (DAD) and UPLC-electrospray ionization multistage/mass spectrometry (ESI-MS/MS) for assuring the feasibility and accuracy. Tested by robustness experiment under slightly changeable conditions, the stability of relative correction factor (RCF) proved to be stable, with RSDs below 5.69%, except for notoginsenoside R1 with relative standard deviation (RSD) 7.83%. This reliable and convenient QAMS method resolved the problem of standard substance insufficiency and improved the quality assessment of preparations consisting of complex compounds with different chemical structures, such as CDPs.

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