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Summary

Radix Isatidis has widely useful activities including anti-virus, anti-bacterial. Tryptanthrin, indigo, and indirubin are active ingredients in R. Isatidis. Response surface methodology (RSM)-optimized infrared-assisted extraction (IRAE) was developed and combined with HPLC for simultaneous determination of tryptanthrin, indigo, and indirubin from R. Isatidis. IRAE were investigated through extraction yields of the three components and optimized by RSM. The optimum conditions were as follows: infrared power of 129 W, solid/liquid ratio of 1:40 g/mL, and irradiation time of 22.5 min. IRAE conditions obtained by RSM were not only accurate, but also had practical value reflecting the expected optimization. Subsequently, this novel IRAE method was evaluated by extraction yield of the components of R. Isatidis samples from different regions. Compared with common extraction methods including maceration extraction (ME), reflux extraction (RE), ultrasound-assisted extraction (UAE), and microwave-assisted extraction (MAE), IRAE showed higher yield with advantages of no limitation of solvent selection, low cost, convenience under optimum extraction conditions. These results suggested the potential of RSM-optimized IRAE for extraction and analysis of the water-/fat-soluble compositions of Chinese herbal medicine. A simple chromatographic separation for simultaneous determination of tryptanthrin, indigo, and indirubin from Chinese herbal medicine R. Isatidis was performed on a C18 column (Diamonsil 150 mm × 4.6 mm i.d., 5 μm) with a mobile phase isocratic consisting of methanol and water at a flow-rate of 0.8 mL min−1. The retention times of tryptanthrin, indigo, and indirubin were 15.4, 31.9, and 58.6 min, respectively. The linear equations were obtained as follows: y = −3094.5744 + 21208.792x for tryptanthrin (R = 0.9998, 0.9–18.0 μg mL−1), y = 4730.0448 + 30180.567x for indigo (R = 0.9997, 0.5–10.0 μg mL−1) and y = −6582.9045 + 67069.312x for indirubin (R = 0.9997, 0.4–8.0 μg mL−1). The result showed that RSM-optimized IRAE was a simple, efficient pretreatment method for the analysis of complex matrix.

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Abstract

Dodecylamine hydrochloride C12H25NH3·Cl(s) and bis-dodecylammonium tetrachlorozincate (C12H25NH3)2ZnCl4(s) were synthesized by the method of liquid phase reaction. The constant-volume energy of combustion of dodecylamine hydrochloride was measured by means of a RBC-II precision rotating-bomb combustion calorimeter at T = (298.15 ± 0.001) K. The standard molar enthalpy of formation of C12H25NH3·Cl(s) was calculated to be (C12H25NH3·Cl, s) = −(706.79 ± 3.97) kJ mol−1 from the constant-volume energy of combustion. In accordance with Hess’ law, a reasonable thermochemical cycle was designed and the enthalpy change of the synthesis reaction of the complex (C12H25NH3)2ZnCl4(s) was determined by use of an isoperibol solution-reaction calorimeter. The standard molar enthalpy of formation of (C12H25NH3)2ZnCl4(s) was calculated as [(C12H25NH3)2ZnCl4, s] = −(1862.14 ± 7.95) kJ mol−1 from the standard molar enthalpy of formation of C12H25NH3·Cl(s) and other auxiliary thermodynamic data.

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A method was developed for the preparative separation of two alkaloids from the crude extract of the radix of Rauvolfia verticillata (Lour.) Baill. in a single run. The two-phase solvent system composed of petroleum ether–ethyl acetate–methanol–water (5:5:2:8, v/v), where triethylamine (40 mmol/L) was added to the upper organic phase as the stationary phase and hydrochloric acid (10 mmol/L) was added to the lower aqueous phase as the mobile phase, was selected for this separation by pH-zone-refining counter-current chromatography (PZRCCC). For the preparative separation, the apparatus was rotated at a speed 850 rpm, while the mobile phase was pumped into the column at 2 mL/min. As a result, 112 mg of reserpine and 21 mg of yohimbine were obtained from 3 g of crude extract in a single run. The analysis of the isolated compounds was determined by high-performance liquid chromatography (HPLC) at 230 nm with purities of over 91.0%, and the chemical identification was carried out by the data of electrospray ionization–mass spectrometry (ESI–MS) and nuclear magnetic resonance (NMR) spectroscopy. The technique introduced in this paper is an efficient method for preparative separation of reserpine and yohimbine from devil pepper radix. It will be beneficial to utilize medicinal materials and also useful for the separation, purification, and pharmacological study of Chinese herbal ingredients.

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Journal of Thermal Analysis and Calorimetry
Authors: F. Xu, L. Sun, P. Chen, Y. Qi, J. Zhang, J. Zhao, Y. Liu, L. Zhang, Zhong Cao, D. Yang, J. Zeng, and Y. Du

Abstract  

The heat capacities of LiNH2 and Li2MgN2H2 were measured by a modulated differential scanning calorimetry (MDSC) over the temperature range from 223 to 473 K for the first time. The value of heat capacity of LiNH2 is bigger than that of Li2MgN2H2 from 223 to 473 K. The thermodynamic parameters such as enthalpy (HH 298.15) and entropy (SS 298.15) versus 298.15 K were calculated based on the above heat capacities. The thermal stabilities of them were investigated by thermogravimetric analysis (TG) at a heating rate of 10 K min−1 with Ar gas flow rate of 30 mL min−1 from room temperature to 1,080 K. TG curves showed that the thermal decomposition of them occurred in two stages. The order of thermal stability of them is: Li2MgN2H2 > LiNH2. The results indicate that addition of Mg increases the thermal stability of Li–N–H system and decrease the value of heat capacities of Li–N–H system.

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Citri Grandis Exocarpium (CGE) is a traditional Chinese medicine with a variety of biological activities. For efficient quality control of CGE, a simple, rapid, and accurate high-performance liquid chromatographic (HPLC) method was developed for simultaneous determination of four main compounds (naringin, rhoifolin, meranzin hydrate, and isoimperatorin) in this herb. These four compounds were separated on a C18 column by gradient elution with methanol and water. The flow rate was 1.0 mL·min−1, and the detection wavelength was 324 nm. The recoveries of the method ranged from 96.32% to 103.71%, and good linear relationships (r 2 > 0.9998) over relative wide concentration ranges were obtained. Then this validated method was successfully applied to the analysis of nine batches of CGE samples.

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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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Journal of Radioanalytical and Nuclear Chemistry
Authors: K. Inn, Zhichao Lin, Zhongyu Wu, C. McMahon, J. Filliben, P. Krey, M. Feiner, Chung-King Liu, R. Holloway, J. Harvey, I. Larsen, T. Beasley, C. Huh, S. Morton, D. McCurdy, P. Germain, J. Handl, M. Yamamoto, B. Warren, T. Bates, A. Holms, B. Harvey, D. Popplewell, M. Woods, S. Jerome, K. Odell, P. Young, and I. Croudace

Abstract  

In 1977, the Low-level Working Group of the International Committee on Radionuclide Metrology met in Boston, MA (USA) to define the characteristics of a new set of environmental radioactivity reference materials. These reference materials were to provide the radiochemist with the same analytical challenges faced when assaying environmental samples. It was decided that radionuclide bearing natural materials should be collected from sites where there had been sufficient time for natural processes to redistribute the various chemically different species of the radionuclides. Over the succeeding years, the National Institute of Standards and Technology (NIST), in cooperation with other highly experienced laboratories, certified and issued a number of these as low-level radioactivity Standard Reference Materials (SRMs) for fission and activation product and actinide concentrations. The experience of certifying these SRMs has given NIST the opportunity to compare radioanalytical methods and learn of their limitations. NIST convened an international workshop in 1994 to define the natural-matrix radionuclide SRM needs for ocean studies. The highest priorities proposed at the workshop were for sediment, shellfish, seaweed, fish flesh and water matrix SRMs certified for mBq per sample concentrations of 90 Sr, 137 Cs and 239 Pu + 240 Pu. The most recent low-level environmental radionuclide SRM issued by NIST, Ocean Sediment (SRM 4357) has certified and uncertified values for the following 22 radionuclides: 40 K, 90 Sr, 129 I, 137 Cs, 155 Eu, 210 Pb, 210 Po, 212 Pb, 214 Bi, 226 Ra, 228 Ra, 228 Th, 230 Th, 232 Th, 234 U, 235 U, 237 Np, 238 U, 238 Pu, 239 Pu + 240 Pu, and 241 Am. The uncertainties for a number of the certified radionuclides are non-symmetrical and relatively large because of the non-normal distribution of reported values. NIST is continuing its efforts to provide the ocean studies community with additional natural matrix radionuclide SRMs. The freeze-dried shellfish flesh matrix has been prepared and recently sent to participating laboratories for analysis and we anticipate receiving radioanalytical results in 2000. The research and development work at NIST produce well characterized SRMs that provide the world's environment-studies community with an important foundation component for radionuclide metrology.

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