Size-selective poorly soluble particulate reference materials for evaluation of quantitative analytical methods

Owing to the absence of readily available certified particulate reference materials (RMs), most analytical methods used to determine particulate contaminant levels in workplace or other environments are validated using solution RMs, which do not assess the robustness of the digestion step for all forms and sizes of particles in a sample. A library of particulate RMs having a range of chemical forms and particle sizes is needed to support a shift in method evaluation strategies to include both solution and particulate RMs. In support of creating this library, we characterized bulk and physically size separated fractions of beryllium oxide (BeO) particles recovered from the machining fluid sludge of an industrial ceramic products grinding operation. Particles were large agglomerates of compact, crystalline BeO primary particles having diameters on the order of several micrometers. As expected, the particle surface area was independent of sieve size, with a range from 3.61 m(2)/g (53-63-microm fraction) to 4.82 m(2)/g (355-600-microm fraction). The density was near the theoretical value (3.01 g/cm(3)). The data support more detailed characterization of the sludge materials for use as size-selective RMs. This work illustrates an approach that can be used to develop RMs that are difficult to digest.     

Reaction of fluorogenic reagents with proteins I. Mass spectrometric characterization of the reaction with 3-(2-furoyl)quinoline-2-carboxaldehyde, Chromeo P465, and Chromeo P503

3-(2-Furoyl)quinoline-2-carboxaldehyde (FQ), Chromeo P465, and Chromeo P503 are weakly fluorescent reagents that react with primary amines to produce fluorescent products. We studied the reaction of these reagents with alpha-lactalbumin by mass spectrometry. The reaction generated a set of products by the addition of one or more labels to the protein. At room temperature, the reaction was an order of magnitude faster with the Chromeo reagents than with FQ; however, the steady-state labeling efficiency was a factor of two higher for FQ compared with the Chromeo reagents. The relative abundance of the products with FQ usually followed a binomial distribution, which suggests that the labeling sites were uniformly accessible to this reagent. In contrast, the distribution of reaction products with the Chromeo reagents did not follow a binomial distribution for reactions performed in the absence of sodium dodecyl sulfate (SDS); it appears that the protein labeled with the Chromeo reagents refolded into a relatively stable secondary structure that hid some reactive sites. The reaction with the Chromeo reagent did follow the binomial distribution if the protein underwent treatment with 1% SDS at 95 degrees C for 5 min, which apparently disrupts the protein's secondary structure and allowed uniform access to all labeling sites. Chromeo 503 labeled seven of the 13 primary amines in denatured alpha-lactalbumin.     

电感耦合等离子体原子发射光谱法测定钛酸钡纳米粉体中7种杂质元素

钛酸钡纳米粉体样品用盐酸溶解,在所得样品溶液中用电感耦合等离子体原子发射光谱法测定了以氧化物存在于样品中的7种杂质元素(包括镁、锶、钾、钠、铝、硅及铁),对测定的光谱条件进行了试验并优化达到上述各元素的测定上限为0.1%(质量分数).测得方法的检出限(3S/b)为(单位μg·L-1):2.0(铝),1.0(铁),20.0(钾),0.2(镁),4.0(钠),3.0(硅)及0.5(锶).应用此方法分析了两件实样,所得结果的相对标准偏差(n=6)小于等于2.0%,对其中4种杂质元素(镁、钾、钠和锶)同时用HG/T 3587-1999标准中的方法作分析校核,所得结果与此方法结果一致.     

Superactivation of the botulinum neurotoxin serotype A light chain metalloprotease: a new wrinkle in botulinum neurotoxin

Small molecules based upon a 2-acylguanidine-5-phenyl thiophene scaffold that can activate the light chain metalloprotease of botulinum neurotoxin serotype A (BoNT LC/A) by an apparent reduction in Km are reported. On the basis of structure-activity relationships and the activation profile, one or more molecules of activator specifically bind to a defined site on the toxin, causing the observed rate enhancement. With the ever-growing clinical uses of BoNT, compounds such as those reported here may provide a method for combating the emerging adaptive immune responses to BoNT.     

A Large Subgraph of the Minimum Weight Triangulation

We present an O(n ⁴ )-time and O(n ² )-space algorithm that computes a subgraph of the minimum weight triangulation (MWT) of a general point set. The algorithm works by finding a collection of edges guaranteed to be in any locally minimal triangulation. We call this subgraph the LMT-skeleton. We also give a variant called the modified LMT-skeleton that is both a more complete subgraph of the MWT and is faster to compute requiring only O(n ² ) time and O(n) space in the expected case for uniform distributions. Several experimental implementations of both approaches have shown that for moderate-sized point sets (up to 350 points^1) the skeletons are connected, enabling an efficient completion of the exact MWT. We are thus able to compute the MWT of substantially larger random point sets than have previously been computed. ^1Though in this paper we summarize some empirical findings for input sets of up to 350 points, a variant of the algorithm has been implemented and tested on up to 40,000 points producing connected subgraphs [2]. Received May 29, 1996, and in revised form January 10, 1997.