A cost effective,sensitive, and environmentally friendly sample preparation method for determination of polycyclic aromatic hydrocarbons in solid samples

A simple, cost effective, and yet sensitive sample preparation technique was investigated for determining Polycyclic Aromatic Hydrocarbons (PAHs) in solid samples. The method comprises ultrasonic extraction, Stir Bar Sorptive Extraction (SBSE), and thermal desorption–gas chromatography–mass spectrometry to increase analytical capacity in laboratories. This method required no clean-up, satisfied PAHs recovery, and significantly advances cost performance over conventional extraction methods, such as Soxhlet and Microwave Assisted Extraction (MAE). This study evaluated three operational parameters for ultrasonic extraction: solvent composition, extraction time, and sample load. A standard material, SRM 1649 a (urban dust), was used as the solid sample matrix, and 12 priority PAHs on the US Environmental Protection Agency (US EPA) list were analyzed. Combination of non-polar and polar solvents ameliorated extraction efficiency. Acetone/hexane mixtures of 2:3 and 1:1 (v/v) gave the most satisfactory results: recoveries ranged from 63.3% to 122%. Single composition solvents (methanol, hexane, and dichloromethane) showed fewer recoveries. Comparing 20 min with 60 min sonication, longer sonication diminished extraction efficiencies in general. Furthermore, sample load became a critical factor in certain solvent systems, particularly MeOH. MAE was also compared to the ultrasonic extraction, and results determined that the 20-min ultrasonic extraction using acetone/hexane (2:3, v/v) was as potent as MAE. The SBSE method using 20 mL of 30% alcohol-fortified solution rendered a limit of detection ranging from 1.7 to 32 ng L⁻¹ and a limit of quantitation ranging from 5.8 to 110 ng L⁻¹ for the 16 US EPA PAHs.     

基于TMS320F240DSP的开关型磁阻电动机调速控制技术

开关型词组电动机调速系统（Switched Reluctance Drive,简称SRD）是80年代中期发展起来的新型交流调速系统，它融新的电动机结构——开关型磁阻电动机（简称SR电动机）与现代电力电子技术，控制技术为一体，兼有异步电动机变频调速系统和直流电动机调速系统的优点，已成为当代电气传动的热门课题之一。     

Tutorial review on validation of liquid chromatography–mass spectrometry methods: Part I

This is the part I of a tutorial review intending to give an overview of the state of the art of method validation in liquid chromatography mass spectrometry (LC–MS) and discuss specific issues that arise with MS (and MS/MS) detection in LC (as opposed to the “conventional” detectors). The Part I briefly introduces the principles of operation of LC–MS (emphasizing the aspects important from the validation point of view, in particular the ionization process and ionization suppression/enhancement); reviews the main validation guideline documents and discusses in detail the following performance parameters: selectivity/specificity/identity, ruggedness/robustness, limit of detection, limit of quantification, decision limit and detection capability. With every method performance characteristic its essence and terminology are addressed, the current status of treating it is reviewed and recommendations are given, how to determine it, specifically in the case of LC–MS methods.     

Determination of polycyclic aromatic hydrocarbons from ambient air particulate matter using a cold fiber solid phase microextraction gas chromatography-mass spectrometry method

Polycyclic aromatic hydrocarbons (PAH) from ambient air particulate matter (PM) were analyzed by a new method that utilized direct immersion (DI) and cold fiber (CF) SPME-GC/MS. Experimental design was used to optimize the conditions of extraction by DI-CF-SPME with a 100μm polydimethylsiloxane (PDMS) fiber. The optimal conditions included a 5min equilibration at 70°C time in an ultrasonic bath with an extraction time of 60min. The optimized method was validated by the analysis of a NIST standard reference material (SRM), 1649b urban dust. The results obtained were in good agreement with certified values. PAH recoveries for reference materials were between 88 and 98%, with a relative standard deviation ranging from 5 to 17%. Detection limits (LOD) varied from 0.02 to 1.16ng and the quantification limits (LOQ) varied from 0.05 to 3.86ng. The optimized and validated method was applied to the determination of PAH from real particulate matter (PM10) and total suspended particulate (TPS) samples collected on quartz fiber filters with high volume samplers.     

Standard operation protocol for analysis of lipid hydroperoxides in human serum using a fully automated method based on solid-phase extraction and liquid chromatography-mass spectrometry in selected reaction monitoring

Standard operating procedures (SOPs) are of paramount importance in the analytical field to ensure the reproducibility of the results obtained among laboratories. SOPs gain special interest when the aim is the analysis of potentially unstable compounds. An SOP for analysis of lipid hydroperoxides (HpETEs) is here reported after optimization of the critical steps to be considered in their analysis in human serum from sampling to final analysis. The method is based on automated hyphenation between solid-phase extraction (SPE) and liquid chromatography-mass spectrometry (LC-MS). The developed research involves: (i) optimization of the SPE and LC-MS steps with a proper synchronization; (ii) validation of the method-viz. accuracy study (estimated as 86.4% as minimum value), evaluation of sensitivity and precision, which ranged from 2.5 to 7.0 ng/mL (0.25-0.70 ng on column) as quantification limit and precision below 13.2%), and robustness study (reusability of the cartridge for 5 times without affecting the accuracy and precision of the method); (iii) stability study, involving freeze-thaw stability, short-term and long-term stability and stock solution stability tests. The results thus obtained allow minimizing both random and systematic variation of the metabolic profiles of the target compounds by correct application of the established protocol.     

Determination of dibenzopyrenes in standard reference materials (SRM) 1649a, 1650, and 2975 using ultrasonically assisted extraction and LC–GC–MS

A method has been developed for analysis of the highly potent polycyclic aromatic hydrocarbon (PAH) carcinogens dibenzo(a,l)pyrene, dibenzo(a,h)pyrene, and dibenzo(a,i)pyrene (molecular weight 302) present in small amounts in diesel and air particulate material. The method can also be used for analysis of the PAH benzo(a)pyrene, coronene, and perylene, for which reference and certified values are available for the standard reference materials used for validation of the method—SRM 1649a (urban dust) and SRM 2975 (diesel particulate matter). The only NIST values that have been published for these dibenzopyrene isomers in the analyzed SRM are reference values for dibenzo(a,i)pyrene and dibenzo(a,h)pyrene in SRM 1649a. The concentrations determined in the SRM were in good agreement with reported NIST-certified and reference values and other concentrations reported in the literature. Standard reference material 1650 (diesel particulate matter) was also analyzed. The method could not, however, be validated using this material because certification of SRM 1650 had expired. The method is based on ultrasonically assisted extraction of the particulate material, then silica SPE pre-separation and isolation, and, separation and detection by hyphenated LC–GC–MS. The method is relatively rapid and requires only approximately 1–5 mg SRM particulate material to identify and quantify the analytes. Low extraction recoveries for the analytes, in particular the dibenzopyrenes, when extracting diesel SRM 2975 and 1650 resulted, however, in the dibenzopyrenes being present in amounts near their limits of quantifications in these samples. The method’s limit of quantification (LOQ), based on analyses of SRM 1649a, is in the range 10–77 pg. By use of this method more than 25 potential PAH isomers with a molecular weight of 302 could be separated.     

基于THS320F2812的开关磁阻电机磁链特性检测

本文研究了开关磁阻电机（SRM）磁链特性实验检测方法,建立了基于DSP芯片TMS320F2812的SRM磁链检测系统,利用ADC模块实时采集不同转子位置的电压、电流信号,将数据传送到上位机,根据间接磁链测量原理,由数字离散方法计算磁链值,得到SRM磁链电流特性曲线和磁链-转子位置-电流模型。     

Characterization of Standard Reference Material 2941, uranyl-ion-doped glass, spectral correction standard for fluorescence

Standard Reference Material^® (SRM^®) 2941 is a cuvette-shaped, uranyl-ion-doped glass, recommended for use for relative spectral correction of emission and day-to-day performance validation of fluorescence spectrometers. Properties of this standard that influence its effective use or contribute to the uncertainty in its certified emission spectrum have been explored here. These properties include its photostability, absorbance, dissolution rate in water, anisotropy, temperature coefficient of fluorescence intensity, and fluorescence lifetimes. The expanded uncertainties in the certified spectrum are about 4% around the peak maximum at 526 nm, using an excitation wavelength of 427 nm. The SRM also exhibits a strong resistance to photodegradation, with no measurable decrease in fluorescence intensity even after 8 h of laser irradiation.     

Study of blood collection and sample preparation for analysis of vitamin D and its metabolites by liquid chromatography–tandem mass spectrometry

The analysis of vitamin D status, with special emphasis on 25-hydroxyvitamin D and 1,25-dihydroxyvitamin D, is gaining interest in clinical studies due to the classical and non-classical effects attributed to this prohormone. In this research, the influence of the two steps preceding determination (viz. sample collection and preparation) on the quantitative analysis of vitamin D and its more important metabolites has been studied. Two preparation approaches, deproteination and solid-phase extraction (SPE), have been evaluated in terms of sensitivity to delimit their application, thus establishing that detection of 1,25-dihydroxyvitamin D cannot be addressed by protein precipitation. Concerning sample collection, serum and plasma reported high accuracy (above 83.3%) for vitamin D and metabolites, while precision, expressed as relative standard deviation, was below 12.9% for all analytes in both samples. Statistical analysis revealed that serum and plasma provided similar physiological levels for vitamin D₃, 24,25-dihydroxyvitamin D₃ and 25-hydroxyvitamin D₃, while significantly different levels were obtained for 1,25-dihydroxyvitamin D₃, always higher in plasma than in serum. Sample collection and treatment have proved to be significant in the analysis of vitamin D and its relevant metabolites.     

Expanding the number of phthalates monitored in house dust

Phthalates have been used as plasticisers for several decades in various industry and consumer products. A method was developed for the determination of 13 not commonly monitored phthalates in household dust. The method was based on solvent extraction using sonication, sample clean-up by solid phase extraction (SPE), and analysis using isotope dilution gas chromatography-tandem mass spectrometry (GC/MS/MS). The method was applied to the analysis of dust samples collected using two vacuum sampling techniques from 38 urban Canadian homes: a sample of fresh or ‘active’ dust (FD) collected by technicians and a composite sample taken from the household vacuum cleaner (HD). Spearman rank correlations between HD and FD samples were significant for six phthalates with median concentrations above their method detection limits (MDLs), suggesting that the HD samples provide comparable results with FD samples. Seven phthalates were detected and quantified in a Canada-wide set of 126 household dust samples, among which six phthalates were detected at frequencies higher than 87%, with median (range) concentrations of 1.9 (<0.42–240) (μg/g) for diisohexyl phthalate (DIHxP), 3.8 (<0.16–260) (μg/g) for di-n-heptyl phthalate (DHepP), 6.6 (<1.1–1170) (μg/g) for diisooctyl phthalate (DIOP), 1.1 (<0.12–390) (μg/g) for di-n-octyl phthalate (DOP), 6.3 (<0.16–430) (μg/g) for dinonyl phthalate (DNP), and 1.8 (<0.18–850) (μg/g) for di-n-decyl phthalate (DDP). High detection frequencies and widely scattered concentration levels of these phthalates in this preliminary set of 126 samples suggested a high variability in potential exposure to phthalates in Canadian homes. NIST SRM 2585 (organic contaminants in house dust) was also analysed; eight phthalates were detected, with concentrations ranging from 6.0 μg/g for DOP to 79 μg/g for DIHxP. The results from SRM 2585 may contribute to the certification of phthalate concentration values in this SRM.