Determination of total dietary fiber in selected foods containing resistant maltodextrin by enzymatic-gravimetric method and liquid chromatography: collaborative study

A method was developed for determination of total dietary fiber (TDF) in foods containing resistant maltodextrin (RMD) which includes nondigestible carbohydrates that are not fully recovered as dietary fiber by conventional TDF methods such as AOAC 985.29 or 991.43. Because the average molecular weight (MW) of RMD is 2000 daltons, lower MW soluble dietary fiber components do not precipitate in 78% ethanol; therefore, RMD is not completely quantitated as dietary fiber by current AOAC methods. The accuracy and precision of the method was evaluated through an AOAC collaborative study. Ten laboratories participated and assayed 12 test portions (6 blind duplicates) containing RMD. The 6 test pairs ranged from 1.5 to 100% RMD. The method consisted of the following steps: (1) The insoluble dietary fiber (IDF) and high MW soluble dietary fiber (HMWSDF) were determined by AOAC 985.29. (2) Ion exchange resins were used to remove salts and proteins contained in the AOAC 985.29 filtrates (including ethanol and acetone). (3) The amount of low MWRMD (LMWRMD) in the filtrates were determined by liquid chromatography. (4) The TDF was calculated by summation of the IDF, HMWSDF, and LMWRMD fractions having nondigestible carbohydrates with a degree of polymerization of 3 and higher. Repeatability standard deviations (RSDr) were 1.33-7.46%, calculated by including outliers, and 1.33-6.10%, calculated by not including outliers. Reproducibility standard deviations (RSDR) were 2.48-9.39%, calculated by including outliers, and 1.79-9.39%, calculated by not including outliers. This method is recommended for adoption as Official First Action.     

New approach to calibrating conductivity meters in the low conductivity range

There is currently a major issue with the calibration of conductivity meters used for high purity water: the lack of availability of a reference material or reference methods for low conductivity ranges (conductivity below 1 S cm^–1 at 25.0 °C, resistivity >1 M cm at 25.0 °C). This paper describes the current status of conductivity measurements in high purity water. A new and improved approach, currently being investigated, should allow us to make the calibration of conductivity meters used for low conductivity ranges traceable to the SI.Milipore, Milli-Q and Elix are registered trademarks of Millipore Corporation.     

Composition and morphology of stack emissions from coal and oil fuelled boilers

Instrumental neutron activation analysis (INAA) together with scanning electron microscopy (SEM) have been used in the study of fly ash from large electric power and heating plants. Two basic kinds of fly ash originating either from brown coal or heavy-oil combustion can be characterized both by morphology and trace element composition. INAA technique used consisted of both short (1 min) and long (2 h) activations to ensure the determination of 30–40 elements in each fly ash sample. The average composition and determination limits obtained by INAA for coal fly ash produced in several electric power plants burning two kinds of brown coal have been compared with those obtained for fly ash originating from heating plants burning heavy-oil. Coal fly ash showed much higher concentrations of many elements especially of Sc. La, Th, Cs, Ce, Sm, Rb and Al in comparison with oil fly ash. On the other hand, the latter contained relatively high concentrations of V and Ni. The results of INAA of fly ash samples can be used for the projection of efficient separating devices and for the evaluation and prediction of contamination levels in the vicinity of large emission sources.     

Oxidative dearomatization of phenols and anilines via lambda(3)- and lambda(5)-iodane-mediated phenylation and oxygenation

Treatment of 2-methylphenols with chloro(diphenyl)-lambda(3)-iodane led to their regioselective dearomatizing 2-phenylation into cyclohexa-2,4-dienone derivatives via a proposed ligand coupling reaction. In the same vein of investigation, treatment of 2-methylanilines with the lambda(5)-iodane 2-iodoxybenzoic acid IBX reagent led to their regioselective dearomatization into previously undescribed ortho-quinol imines.     

Determination of enantiomeric excess and degree of hydrogenation in the enantioselective hydrogenation of ketopantolactone

Summary A new gas chromatographic method for the simultaneous determination of the degree of hydrogenation of ketopantolactone and the enantiomeric excess of pantolactone does not require any derivatisation.

---

Bestimmung von Enantiomerenüberschuß und Hydriergrad bei der enantioselektiven Hydrierung von Ketopantolacton (Kurze Mitt.)

Zusammenfassung Zur Bestimmung des Hydriergrads von Ketopantolacton und des Enantiomerenüberschusses von Pantolacton wird ein neues gaschromatographisches Verfahren eingesetzt, das keine Derivatisierung erfordert.

     

Deprotonation-electrophile trapping of terminal epoxides

Organolithium-induced deprotonation of terminal epoxides in the presence of appropriate diamine ligands allows trapping with a range of electrophiles, yielding functionalised di- and tri-substituted epoxides in good yields and with control of stereochemistry at the epoxide.     

Synthetic application of a substituent controlled claisen rearrangement. Preparation of advanced chiral intermediates for the synthesis of pseudomonic acids

A substituent controlled Claisen rearrangement is employed as the key reaction for a facile construction of chiral intermediates for the synthesis of pseudomonic acids from diacetyl-L-arabinal.     

Radioanalytical quality control of11C,18F and123I-labelled compounds and radiopharmaceuticals

Radiochemical quality control using high performance high pressure liquid chromatography and, to some extent, gas chromatography is described for a variety of carrier-free¹¹C-,¹⁸F-and¹²³I-labelled compounds and radiopharmaceuticals. The particular problems associated with the handling of carrier-free compounds labelled with short-lived radionuclides are outlined, and chromatographic data are given for the separation and purification of such products.