不同消解方法对青钱柳茶叶中6种有益元素含量的影响

目的 测定青钱柳茶叶中6种有益元素的含量,并比较3种消解方法对所测元素的含量影响。方法 青钱柳茶叶样品分别经干法消解、湿法消解、石墨消解处理后,用电感耦合等离子体发射光谱法（ICP-OES）同时测定Ca、K、Mg、Mn、Zn、Cu 6种元素含量,并进行方法学考察。结果 3种消解方法测得的6种元素R²为0.998 8~0.999 9,RSD为0.1%~5.2%,回收率为82.4%~101.8%,均符合测定要求。青钱柳茶叶中Ca、K、Mg、Zn元素含量丰富;湿法消解具有优越性,Ca、K宜选用湿法,Mg、Mn 3种方法均可,Zn宜选用干法和湿法,Cu宜选用干法消解。结论 湿法消解相较干法消解、石墨消解具有优越性,石墨消解作为新兴的消解技术具有很大开发潜力。     

电感耦合高频等离子体发射光谱法测定蒙药角茴香中的微量元素

目的建立电感耦合高频等离子体发射光谱(ICP-OES)法测定蒙药角茴香中Al,As,B,Ba,Cd,Co,Cu,Fe,Hg,In,Mn,Pb,Sr,Zn等14种微量元素含量的测定方法。方法采用微波消解法前处理样品,电感耦合高频等离子体发射光谱(ICP-OES)法测定蒙药角茴香中14种微量元素含量。结果该方法检出限为0.0002～0.006μg.ml-1,各元素加标回收率在95.6%～109.26%之间,RSD小于4.46%。结论该方法可快速、灵敏、准确测定蒙药角茴香中多种微量元素含量。     

Airway drug pharmacokinetics via analysis of exhaled breath condensate

Although the airway surface is the anatomic target for many lung disease therapies, measuring drug concentrations and activities on these surfaces poses considerable challenges. We tested whether mass spectrometric analysis of exhaled breath condensate (EBC) could be utilized to non-invasively measure airway drug pharmacokinetics and predicted pharmacological activities.Mass spectrometric methods were developed to detect a novel epithelial sodium channel blocker (GS-9411/P-680), two metabolites, a chemically related internal standard, plus naturally occurring solutes including urea as a dilution marker. These methods were then applied to EBC and serum collected from four (Floridian) sheep before, during and after inhalation of nebulized GS-9411/P-680. Electrolyte content of EBC and serum was also assessed as a potential pharmacodynamic marker of drug activity. Airway surface concentrations of drug, metabolites, and electrolytes were calculated from EBC measures using EBC:serum urea based dilution factors.GS-9411/P-680 and its metabolites were quantifiable in the sheep EBC, with peak airway concentrations between 1.9 and 3.4 μM measured 1 h after inhalation. In serum, only Metabolite #1 was quantifiable, with peak concentrations ∼60-fold lower than those in the airway (45 nM at 1 h). EBC electrolyte concentrations suggested a pharmacological effect; but this effect was not statistical significant.Analysis of EBC collected during an inhalation drug study provided a method for quantification of airway drug and metabolites via mass spectrometry. Application of this methodology could provide an important tool in development and testing of drugs for airways diseases.     

健康大学生指甲中微量元素Fe Zn Cu Mn含量分析

收集健康大学生的指甲,采用微波消解、电感耦合等离子体发射光谱仪(ICP-OES)测定指甲中微量元素的含量。结果显示指甲中Fe,Zn,Cu,Mn的含量分别为39.12±57.89μg/g,118.83±30.40μg/g,7.11±4.24μg/g和0.66±0.78μg/g。指甲中Fe含量女性显著低于男性(P<0.05)。方法简便、灵敏、准确,结果较好地反映了在校大学生的健康状况,同时也为指甲作为生物样本的可行性提供基础数据。     

元素分析法在中药产品质量监控中的应用

目的：建立参灵草（JSLCC）口服液中元素的检测方法,进而对JSLCC口服液的元素分布情况进行初步探讨,为进一步制订该产品的元素含量质量标准探明方向。方法采用微波消解法对样品进行前处理,以电感耦合等离子体原子发射光谱法（ICP-OES）同时测定JSLCC口服液中各种元素的含量。结果通过57种元素盲扫,确定了JSLCC口服液中含有P、Ni、Mn、B、Mg、Ca、Sr、Ba、Na及K这10种元素,并对其中含量较高的P、Mg、Ca、Sr、Na及K元素进行了定量测定。方法学检测结果显示,P、Mg、Ca、Sr、Na及K元素含量相对标准偏差在1.234%-6.739%之间,回收率在97.615%-108.393%范围内,各元素检出限在0.0000159-0.0182656 mg/L之间。结论本法准确度高,重现性好,检测限低,可满足日常检测需要,初步确定了JSLCC口服液中各元素的含量分布范围。     

Comparison of dry, wet and microwave digestion methods for the multi element determination in some dried fruit samples by ICP-OES

The aim of this study was used to investigate the level of trace metals (Ba, Pb, Cd, Mn, Cr, Co, Ni, Cu, Mn, Zn, Sr and Fe) in some dried fruits (Prunus domestica L., Ficus carica L., Morus alba L., Vitis vinifera L., Prunus armeniaca L., and Malus domestica) samples from Turkey. Trace elements were determined by ICP-OES after dry, wet and microwave digestion methods in dried fruit samples. Validation of the proposed method was carried out by using a NIST-SRM 1515-Apple Leaves certified reference material. Element concentrations in dried fruit samples were 0.33–1.77 (Ba), 0.12–0.54 (Cd), 0.25–1.03 (Co), 0.45–2.30 (Cr), 0.43–2.74 (Cu), 0.56–4.87 (Mn), 0.61–2.54 (Ni), 0.40–2.14 (Pb), 2.16–6.54 (Zn), 0.83–12.02 (Al), 11.82–40.80 (Fe) and 0.16–6.34 (Sr) μg/g. The analytical parameters show that the microwave oven digestion procedure provided best results as compared to the wet and dry digestion procedures. The results were compared with the literature values.     

Comparison of the chemical composition of British and Continental European bottled waters by multivariate analysis

The elemental composition of 37 bottled waters from the UK and continental Europe has been determined. Ca, K, Mg, Na, Al, As, Ba, Cd, Cr, Co, Cu, Fe, Mn, Mo, Ni, Pb, Sb, Sr, U, V and Zn were determined by ICP-OES and ICP-MS, in addition to inorganic and total organic carbon. The composition of all the waters analysed fell within the guideline values recommended by the World Health Organization. Na, Ca, Sr and Ba showed the widest variation in concentrations, ranging over two orders of magnitude. Levels of Fe were below the limit of detection (30 μg L⁻¹) in all samples analysed. Waters produced in the UK generally showed lower levels of most major elements and trace metals, with the exception of Ba (up to 455 μg L⁻¹). Italian waters showed the highest concentrations of Sr (3000–8000 μg L⁻¹) and U (8–13 μg L⁻¹), whereas waters produced in Slovakia and the Czech Republic showed the highest levels of Pb (0.7–4 μg L⁻¹). The use of multivariate analysis reveals an association between high alkaline metal content and high concentrations of As and Cr. There also appears to be a correlation between high Ca and Sr content and high levels of U. Analysis of variance (ANOVA) indicates that the composition of bottled water can be distinguished primarily by the country of origin, over other factors including the geological environment of the source. This would suggest that composition reflects, and is biased towards, consumer preferences.     

Localized Hyperthermia with Iron Oxide–Doped Yttrium Microparticles: Steps toward Image-Guided Thermoradiotherapy in Liver Cancer

PurposeTo test whether iron oxide (IO)–containing yttrium aluminosilicate (YAS) microparticles (MPs) can generate localized therapeutic hyperthermia (≥ 43°C) when injected intratumorally in an animal model of liver cancer and whether MP distributions could be visualized with magnetic resonance (MR) imaging.Materials and MethodsTwenty-one Sprague–Dawley rats implanted with N1-S1 liver tumors were assigned to alternating magnetic field (AMF) exposure following intratumoral injection with IO-YAS MPs (n = 7), sham surgery (n = 7), or baseline iron quantification (n = 7). Three fiberoptic probes allowed spatial and temporal monitoring of temperatures during 24 minutes of AMF exposure. T2-weighted turbo spin-echo MR imaging was performed within 1 hour after the procedure to detect signal voids caused by IO-YAS deposition. Hematoxylin and eosin–stained pathologic slides were also obtained, and the presence of IO-YAS was evaluated with inductively coupled plasma optical emission spectroscopy.ResultsFollowing AMF exposure, intratumoral temperatures after IO-YAS MP injection achieved therapeutic hyperthermia whereas those after sham surgery did not (46.6°C ± 1.3 vs 36.8°C ± 0.4; P < .0001). Within the treated group, the normal hepatic parenchyma (NHP) and rectal temperatures were 37.4°C ± 0.9 and 36.5°C ± 1.0 (P = .0809) at the conclusion of AMF exposure, respectively. A T2-weighted signal void at the tumor site was observed in all seven treated animals, and intratumoral IO-YAS was visualized on subsequent histopathologic examination in each case. The mean ratio of tumor:NHP Fe concentrations attributable to IO-YAS MPs was 108:1.ConclusionsAMF exposure of intratumoral IO-YAS MPs generates localized therapeutic hyperthermia in an animal model of liver cancer. MR detectability and potential for combination brachytherapy warrants further investigation for thermoradiotherapy in liver cancer.     

ICP-OES法与AAS法在质控滤膜多金属测定中的应用比较

目的比较分析2种方法在滤膜金属检测中的应用,评价2种方法的实用性和可靠性。方法分别用2种方法对质控滤膜中的铅、镉、锰、锌进行检测,检测结果采用统计学分析。结果对2种方法最低检出限、测定下限进行比较,ICP-OES法均低于AAS法,2种方法测定滤膜样品结果经配对t检验差异无统计学意义(P0.05)。结论 ICP-OES法灵敏度高于AAS法,且仪器操作简便,分析速度快,可多种元素同时测定,线形范围宽,结果准确可靠,更适用于大批量样品的检验。     

Validation of an ICP-OES method for macro and trace element determination in Laminaria and Porphyra seaweeds from four different countries

An Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) method for speedy simultaneous determination of 12 elements (Al, Ba, Ca, Cu, Fe, K, Mg, Mn, Na, P, Sr and Zn) in seaweeds used as human food was optimized and then validated according to Eurachem guidelines. First, instrumental parameters (nebulizer argon flow rate and incident power) were optimized and then analytical lines free from spectral interferences were selected. The method was validated using biological Certified Reference Materials (CRMs). Intra- and inter-assay precision varied from 0.79% to 5.74% and from 2.48% to 8.57%, respectively, depending on the element studied. Within the experimental error, concentrations measured for each element coincided with certified values. Sensitivities, linearity and detection and quantification limits were also determined. Samples of seaweeds (Porphyra and Laminaria) from France, Spain, Korea and Japan were analyzed by using the optimized and validated method. Some considerations on element composition of analyzed samples were made. Seaweeds from the Korean and Japanese coasts tended to display the highest concentrations of P and Al. In contrast, French Porphyra samples showed the lowest levels of Ba, Cu, Fe and Mn. Because great differences in element concentrations were observed due to costal origin and genus, any generalization regarding the algal mineral content may be considered misleading and scientifically inappropriate.