Determination of ethyl glucuronide in hair samples of Chinese people by protein precipitation (PPT) and large volume injection-gas chromatography-tandem mass spectrometry (LVI-GC/MS/MS)

Ethyl glucuronide (EtG) has been shown to be a suitable marker of excessive alcohol consumption. Determination of EtG in hair samples may help to differentiate social drinkers from alcoholics, and this testing can be widely used in forensic science, treatment programs, workplaces, military bases as well as driving ability test to provide legal proof of drinking. A method for determination of EtG in hair samples using large volume injection-gas chromatography-tandem mass spectrometry (LVI-GC/MS/MS) was developed and validated. Hair samples (in 1 mL deionized water) were ultrasonicated for 1h and incubated overnight; these samples were then deproteinated to remove impurities and derivatisated with 15 μL of pyridine and 30 μL of BSTFA. EtG was detected using GC/MS/MS in multiple-reaction monitoring mode. This method exhibited good linearity: y=0.0036 x+0.0437, R2=0.9993, the limit of detection and the limit of quantification were 5 pg/mg and 10 pg/mg, respectively. The extraction recoveries were more than 60%, and the inter-day and intra-day relative standard deviations (RSD) were less than 15%. This method has been applied to the analysis of EtG in hair samples from 21 Chinese subjects. The results for samples obtained from all of those who were teetotallers were negative, and the results for the other 15 samples ranged from 10 to 78 pg/mg, except for one negative sample. These data are the basis for interpretation of alcohol abuse.     

Post‐chemiluminescence determination of chloramphenicol based on luminol–potassium periodate system

A post‐chemiluminescence (PCL) phenomenon was observed when chloramphenicol was injected into a mixture of luminol and potassium periodate after the chemiluminescence (CL) reaction of luminol–potassium periodate had finished. The possible reaction mechanism was proposed based on studies of the CL kinetic characteristics, the CL spectra, the fluorescence spectra and the UV‐vis absorption spectra of the related substances. Based on the PCL reaction, a rapid and sensitive method for the determination of chloramphenicol was established. The linear response range was 6.0 × 10^?7–1.0 × 10^?5 mol/L, with a correlation coefficient of 0.9986. The relative standard deviation (RSD) for 5.0 × 10^?6 mol/L chloramphenicol was 2.3% (n = 11). The detection limit was 1.6 × 10^?7 mol/L. The method has been applied to the determination of chloramphenicol in pharmaceutical samples with satisfactory results. Copyright © 2011 John Wiley & Sons, Ltd.     

Flow‐injection chemiluminescence method for the determination of chloramphenicol based on luminol–sodium periodate order‐transform second‐chemiluminescence reaction

A new chemiluminescence (CL) reaction was observed when chloramphenicol solution was injected into the mixture after the end of the reaction of alkaline luminol and sodium periodate or sodium periodate was injected into the reaction mixture of chloramphenicol and alkaline luminol. This reaction is described as an order‐transform second‐chemiluminescence (OTSCL) reaction. The OTSCL method combined with a flow‐injection technique was applied to the determination of chloramphenicol. The optimum conditions for the order‐transform second‐chemiluminescence emission were investigated. A mechanism for OTSCL has been proposed on the basis of the chemiluminescence kinetic characteristics, the UV‐visible spectra and the chemiluminescent spectra. Under optimal experimental conditions, the CL response is proportional to the concentration of chloramphenicol over the range 5.0 × 10^?7–5.0 × 10^?5 mol/L with a correlation coefficient of 0.9969 and a detection limit of 6.0 × 10^?8 mol/L (3σ). The relative standard deviation (RSD) for 11 repeated determinations of 5.0 × 10^?6 mol/L chloramphenicol is 1.7%. The method has been applied to the determination of chloramphenicol in pharmaceutical samples with satisfactory results. Copyright © 2011 John Wiley & Sons, Ltd.     

比索洛尔联合丹红注射液治疗老年心肌缺血的临床疗效

目的:探讨比索洛尔联合丹红注射液对老年心肌缺血患者血清肌钙蛋白、心肌酶水平及临床疗效的影响。方法:收集我院收治的老年心肌缺血患者58例,随机分为观察组和对照组,每组各29例。所有患者均给予调脂、抗血小板和抗心肌缺血等基础治疗。对照组患者给予丹红注射液静脉滴注,观察组在对照组基础上给予比索洛尔治疗。观察并比较两组患者治疗前后的心肌酶(CK、CK-MB、AST、LDH)、血清肌钙蛋白I(c Tn I)、肿瘤坏死因子-α(TNF-α)水平及临床疗效。结果:与治疗前相比,两组患者治疗后心肌酶(CK、CK-MB、AST、LDH)、血清肌钙蛋白I(c Tn I)及肿瘤坏死因子-α(TNF-α)水平降低(P0.05);与对照组比较,观察组患者心肌酶(CK、CK-MB、AST、LDH)、血清肌钙蛋白I(c Tn I)及肿瘤坏死因子-α(TNF-α)水平较低(P0.05),临床总有效率较高(P0.05)。结论:比索洛尔联合丹红注射液对老年心肌缺血有较好的临床疗效。     

Highly luminescent S,N co‐doped carbon quantum dots‐sensitized chemiluminescence on luminol–H2O2 system for the determination of ranitidine

S,N co‐doped carbon quantum dots (N,S‐CQDs) with super high quantum yield (79%) were prepared by the hydrothermal method and characterized by transmission electron microscopy, photoluminescence, UV–Vis spectroscopy and Fourier transformed infrared spectroscopy. N,S‐CQDs can enhance the chemiluminescence intensity of a luminol–H₂O₂ system. The possible mechanism of the luminol–H₂O₂–(N,S‐CQDs) was illustrated by using chemiluminescence, photoluminescence and ultraviolet analysis. Ranitidine can quench the chemiluminescence intensity of a luminol–H₂O₂–N,S‐CQDs system. So, a novel flow‐injection chemiluminescence method was designed to determine ranitidine within a linear range of 0.5–50 μg ml^?1 and a detection limit of 0.12 μg ml^?1. The method shows promising application prospects.     

简易注气法测定刺槐木质部导管组织长度

导管组织在木本植物水力学特性及水分关系中的作用逐渐受到关注,但其长度的传统测试装置和方法相对繁琐。本研究在注气法原理基础上进行改进,改进后装置简易、操作便捷。结果表明,本方法可以成功测定刺槐(Robinia pseudoacacia L.)导管的长度及相关参数:气体传导耗散系数为0.111±0.012;最大导管长度为56.9±1.5 cm;平均导管长度为19.6±2.5 cm;最大分布导管长度为9.8±1.3 cm。枝条注气方向对测试结果没有明显影响。测试过程中注气端压强变化不明显,对导管长度及相关参数的测定和计算影响不显著。本方法与传统注气法相比具有更高的精确度。     

Stability of Prussian Blue in Soils of a Former Manufactured Gas Plant Site

Soil contamination with iron-cyanide complexes is a common problem at former manufactured gas plant (MGP) sites. Dissolution of the cyanide, from Prussian Blue (ferric ferrocyanide), creates an environmental hazard, whereas the risk of groundwater contamination depends on the stability of dissolved iron–cyanide complexes. Lack of a standard leaching method to determine the water-soluble (plant-available) cyanide fraction generates potential limitations for implementing remediation strategies like phytoremediation. Applicability of neutral solution extraction to determine the water-soluble cyanide fraction and the stability of Prussian Blue in surface and near-surface soils of an MGP site in Cottbus, undersaturated and unsaturated water conditions, was studied in column leaching and batch extraction experiments. MGP soils used in the long-term tests varied according to the pH (5.0–7.7) and the total cyanide content (40–1718 mg kg^?1). Column leaching, after four months of percolation, still yielded effluent concentrations exceeding the German drinking water limit (> 50 μg L^?1) and the solubility of Prussian Blue reported in the literature (< 1 mg L^?1) from both alkaline and acidic soils. Long-term (1344 h) extraction of MGP soils with distilled water was sufficient to dissolve 97% of the total cyanide from the slightly alkaline soils and up to 78% from the acidic soils. Both experiments revealed that dissolution of ferric ferrocyanide under circum-neutral pH and oxic water conditions is a function of time, where the released amount is dependent on the soil pH and total cyanide content. Unexpectedly high and continuous solubility of Prussian Blue, both in acidic and slightly alkaline MGP soils, implies the need to introduce an additional cyanide fraction (“readily soluble fraction”) to improve and specify cyanide leaching methods. Long-term extraction of cyanide-contaminated soil in neutral solution seems to be a promising approach to evaluate the potential hazard of groundwater pollution at the MGP sites.     

Imaging Intracellular Ca2+ Signals in Striatal Astrocytes from Adult Mice Using Genetically-encoded Calcium Indicators

Astrocytes display spontaneous intracellular Ca²⁺ concentration fluctuations ([Ca²⁺]_i) and in several settings respond to neuronal excitation with enhanced [Ca²⁺]_i signals. It has been proposed that astrocytes in turn regulate neurons and blood vessels through calcium-dependent mechanisms, such as the release of signaling molecules. However, [Ca²⁺]_i imaging in entire astrocytes has only recently become feasible with genetically encoded calcium indicators (GECIs) such as the GCaMP series. The use of GECIs in astrocytes now provides opportunities to study astrocyte [Ca²⁺]_i signals in detail within model microcircuits such as the striatum, which is the largest nucleus of the basal ganglia. In the present report, detailed surgical methods to express GECIs in astrocytes in vivo, and confocal imaging approaches to record [Ca²⁺]_i signals in striatal astrocytes in situ, are described. We highlight precautions, necessary controls and tests to determine if GECI expression is selective for astrocytes and to evaluate signs of overt astrocyte reactivity. We also describe brain slice and imaging conditions in detail that permit reliable [Ca²⁺]_i imaging in striatal astrocytes in situ. The use of these approaches revealed the entire territories of single striatal astrocytes and spontaneous [Ca²⁺]_i signals within their somata, branches and branchlets. The further use and expansion of these approaches in the striatum will allow for the detailed study of astrocyte [Ca²⁺]_i signals in the striatal microcircuitry.     

Modified carbon paste electrodes for flow injection amperometric determination of isocitrate dehydrogenase activity in serum

A carbon paste electrode modified with the adsorbed products of the electrochemical oxidation of adenosine triphosphate is described. The electrode was applied to the amperometric electrocatalytic detection of the reduced form of both nicotinamide adenine dinucleotide and nicotinamide adenine dinucleotide phosphate. The catalytic oxidation current shows a linear dependence on the concentration of the reduced form of nicotinamide adenine dinucleotide up to 1x10(-4)M, with a detection limit of 5x10(-9)M. Modified carbon paste electrodes were coated with an electrogenerated film of nonconducting poly(o-phenylenediamine) to obtain a stable amperometric response for at least 150h. In addition to static measurements, determination of both reduced cofactors was carried out in a flow injection analysis system with a thin-layer amperometric detection cell. The electrocatalytic monitoring of reduced nicotinamide adenine dinucleotide phosphate was applied to flow injection measurement of isocitrate dehydrogenase activity in serum. The results were in good agreement with those for the standard spectrophotometric test kit. The proposed method consumed less time and reagents and provided better precision than the standard method.     

Flow‐injection chemiluminescence method to detect a β2 adrenergic agonist

A new method for the detection of β₂ adrenergic agonists was developed based on the chemiluminescence (CL) reaction of β₂ adrenergic agonist with potassium ferricyanide–luminol CL. The effect of β₂ adrenergic agonists including isoprenaline hydrochloride, salbutamol sulfate, terbutaline sulfate and ractopamine on the CL intensity of potassium ferricyanide–luminol was discovered. Detection of the β₂ adrenergic agonist was carried out in a flow system. Using uniform design experimentation, the influence factors of CL were optimized. The optimal experimental conditions were 1 mmol/L of potassium ferricyanide, 10 µmol/L of luminol, 1.2 mmol/L of sodium hydroxide, a flow speed of 2.6 mL/min and a distance of 1.2 cm from ‘Y₂’ to the flow cell. The linear ranges and limit of detection were 10–100 and 5 ng/mL for isoprenaline hydrochloride, 20–100 and 5 ng/mL for salbutamol sulfate, 8–200 and 1 ng/mL for terbutaline sulfate, 20–100 and 4 ng/mL for ractopamine, respectively. The proposed method allowed 200 injections/h with excellent repeatability and precision. It was successfully applied to the determination of three β₂ adrenergic agonists in commercial pharmaceutical formulations with recoveries in the range of 96.8–98.5%. The possible CL reaction mechanism of potassium ferricyanide–luminol–β₂ adrenergic agonist was discussed from the UV/vis spectra. Copyright © 2014 John Wiley & Sons, Ltd.