On-line preconcentration/determination of copper in parenteral solutions using activated carbon by inductively coupled plasma optical emission spectrometry

A method for the on-line preconcentration of copper using a minicolumn packed with activated carbon and its subsequent determination by inductively coupled plasma optical emission spectrometry (ICP-OES) coupled with flow injection (FI) was studied. In order to determinate the copper concentration present in parenteral solutions; it was retained on activated carbon (AC) at pH 9.5. A sensitivity enrichment factor of 30-fold was obtained with respect to the copper determination by ICP-OES without preconcentration. The detection limit for the preconcentration of 25 ml of sample was 0.1 microgl(-1). The precision for the ten replicate determinations at the 2.5 microgl(-1) Cu level was 3.0% relative standard deviation (R.S.D.), calculated with the peak heights. The calibration graph using the preconcentration method for cooper species was linear with a correlation coefficient of 0.9996 at levels near the detection limits up to at least 200 microgl(-1). The method was successfully applied to the determination of copper in parenteral solutions.     

Cinchocaine hydrochloride determination by atomic absorption spectrometry and spectrophotometry

Two sensitive spectrophotometric and atomic absorption spectrometric procedures have been developed for determination of cinchocaine hydrochloride (Cin.Cl) in pure form and in pharmaceutical formulation. The spectrophotometric method was based on formation of an insoluble colored ion-associate between the cited drug and tetrathiocyanatocobaltate (CoTC) or hexathiocyanatochromate (CrTC) which dissolved and extracted in an organic solvent. The optimal experimental conditions for quantitative extraction such as pH, concentration of the reagents and solvent were studied. Toluene and iso-butyl alcohol proved to be the most suitable solvents for quantitative extraction of Cin-CoTC and Cin-CrTC ion-associates with maximum absorbance at 620 and 555 nm, respectively. The optimum concentration ranges, molar absorptivities, Ringbom ranges and Sandell sensitivities were also evaluated. The atomic absorption spectrometric method is based on measuring of the excess cobalt or chromium in the aqueous solution, after precipitation of the drug, at 240.7 and 357.9 nm, respectively. Linear application ranges, characteristic masses and detection limits were 57.99-361.9, 50.40 and 4.22 microg ml(-1) of Cin.Cl, in case of CoTC, while 37.99-379.9, 18.94 and 0.81 microg ml(-1) in case of CrTC.     

原子吸收分光光度法测定肾骨颗粒中钙的含量

目的:建立肾骨颗粒中钙的含量测定的方法,为其质量评价提供理论依据。方法:采用原子吸收分光光度法对肾骨颗粒中的钙的含量进行测定,并将结果与化学滴定法进行比较。结果:该方法线性、精密度、准确度、范围、耐用性均良好,钙高、中、低含量的加样回收率分别为100.20%,99.14%,99.62%(n=9)。结论:该方法灵敏快速,准确可靠,可用于肾骨颗粒中钙含量的测定。     

采用原子吸收分光光度法测定药用辅料硬脂富马酸钠中的重金属铅含量

目的建立石墨炉-原子吸收分光光度法测定硬脂富马酸钠中铅含量。方法硬脂富马酸钠经微波消解,赶酸后,按照拟定的仪器工作条件,采用石墨炉-原子吸收分光光度法测定硬脂富马酸钠中铅含量。结果铅元素在0~100μg·L~(-1)内与峰面积呈良好的线性关系(r=0.9999);高、中、低3个浓度平均回收率分别为96.8%、103.4%、92.1%,RSD分别为6.2%、1.3%、4.4%,说明本法准确度较好。结论本方法准确度高、重现性好,可用于硬脂富马酸钠中铅的含量测定,为建立药用辅料硬脂富马酸钠的质量标准提供参考。     

原子吸收分光光度法测定局方至宝丸中可溶性汞盐的含量

目的建立测定局方至宝丸中可溶性汞盐的含量。方法采用原子吸收分光光度法,测定波长253.6 nm,测定时间4.0 s,载气流速为200 mL·min~(-1),氘灯作为背景校正。结果样品的加样回收率为99.2%~102.8%,RSD为1.1%~4.2%。结论建立的方法具有准确度高,稳定性、重复性好等优点,可以用于局方至宝丸中可溶性汞盐的含量控制。     

塞曼火焰原子吸收与石墨炉原子吸收法测定明胶空心胶囊壳中铬的方法比较

目的:研究塞曼效应背景校正的火焰和石墨炉原子吸收法测定胶囊中铬的影响。方法:采用微波消解仪对胶囊壳样品进行消解,在波长359.3 nm下,灯电流7.5 mA;狭缝宽1.3 nm,塞曼背景校正,分别采用塞曼火焰原子吸收和石墨炉原子吸收法进行测定。结果:火焰原子吸收法:线性范围0.04～1.0 mg.mL-1;相关系数为0.9998,检测限5.26 ng.mL-1,RSD为0.68%～1.0%,加样回收率为100.0%～116.7%;石墨炉原子吸收法:线性范围为1～20 ng.mL-1,相关系数为0.9998,检测限为0.26 ng.mL-1,RSD为1.7%～4.9%,加样回收率为98.2%～105.6%。结论:塞曼火焰原子吸收法简便、快捷,能满足大量样品筛选及企业内部质控筛选与定值;石墨炉原子吸收法检测限较前者低,准确度较高。     

石墨炉原子吸收分光光度法测定大鼠血浆和尿液中的赛特铂

目的建立大鼠血浆和尿液中赛特铂含量测定的无火焰石墨炉原子吸收分光光度法。方法采用岛津AA-670原子吸收分光光度仪及GFA-4A石墨炉,上海电光KY-1铂空心阴极灯,检测波长265.9 nm,测定大鼠血浆和尿液中的赛特铂含量。血尿样品用Triton X-100稀释,进样50μL。结果在浓度范围0.25 mg.L-1~10.0 mg.L-1内,样品峰面积与浓度呈良好线性关系,相关系数r2分别为血浆0.9952,尿液0.9878;加样回收率为血浆89%~112%,尿液82%~100%。结论方法简便可靠,适于生物样本中的赛特铂含量测定和动物药动学研究。     

石墨炉原子吸收分光光度法测定大鼠血浆和尿液中的赛特铂

OBJECTIVE To develop a rapid,accurate and sensitive method for the measurements of satraplatin in biological fluids of rats.METHODS Satraplatin in plasma and urine was analyzed by flameless atomic absorption spectrometry on an instrument Shimadzu AA-670 a     

磁性固相萃取结合火焰原子吸收光谱法测定河水中铬离子的含量

目的合成离子液体负载修饰磁性纳米材料,建立磁性固相萃取-火焰原子吸收分光光度法(magnetic solid phase extraction-flame atomic absorption spectrophotometry,MSPE-FAAS)测定河水中铬离子(Cr~(6+))的含量。方法采用两步合成法,以Fe_3O_4、原硅酸四乙酯(tetrathoxysilane,TEOs)合成中间产物Fe_3O_4@SiO_2,再将其和1-烷基-3-甲基咪唑六氟磷酸盐合成Fe_3O_4@SiO_2@CnMIM PF_6即系列离子液体负载修饰磁性纳米材料。将150 mg上述材料加至过滤后的河水样品(用盐酸溶液调p H值至6.0)100 m L中,振荡10 min,静置20 min,当磁铁分离时,去除上清液,用5 m L浓度为1 mol·L-1的HCl溶液洗脱,采用火焰原子吸收分光光度法在波长357.9 nm下对洗脱液中的六价铬离子进行含量测定。结果通过红外分光光度法(infrared spectroscopy,IR)、扫描电镜法(scanning electron microscope,SEM)、热重分析法(thermogravimetric analysis,TGA)和X-射线衍射法(X-ray diffraction,XRD)对离子液体修饰磁性纳米材料Fe_3O_4@SiO_2@C6M IM PF6进行表征。在优化条件下,采用火焰原子吸收分光光度法(flame atomic absorption spectrophotometry,FAAS)对河水中的铬离子(Cr~(6+))进行含量测定,检测限为质量浓度6.5μg·L~(-1),加样回收率为94.5%~100.5%,RSD在2.5%~3.6%内。结论该方法适用于河水中铬离子(Cr~(6+))的含量测定。     

石墨炉原子吸收法测定螺旋藻中铅含量的不确定度评定

目的评定用原子吸收光谱法测定螺旋藻中铅含量的不确定度。方法按GB/T5009.12-2010食品中铅的测定第一法石墨炉原子吸收光谱法测定。结果对测量结果主要影响因素引起的不确定度进行了逐个分析、评定。结论该评定思路清晰,主要评定影响因素有重复性、重现性、标准溶液、溶液体积、检测仪器等,适用于原子吸收光谱法测定食品中的元素含量分析的不确定度评定。     

Simple determination of tin in biological materials by atomic absorption spectrometry with a graphite furnace

A simple and rapid determination of tin in biological materials (blood, brain, liver, kidney, etc,) by atomic absorption spectrometry (AAS) with a graphite furnace is described. Suppression of interferences by direct addition of ascorbic acid in wet-ashed biological materials was investigated for the determination of tin. This method involves no extraction with organic solvent for removal of the interferences, and therefore it is neither time consuming nor error prone, and is suitable for large sample sizes and small sample volumes. The limit of detection of this method is 0.002 microgram/mL, equivalent to a limit of detection in the materials of 0.02 microgram/g. The calibration graph is linear up to 1 microgram/mL of tin.     

流动注射氢化物发生原子吸收光谱法测定多种微量元素注射液中硒含量

目的建立多种微量元素注射液Ⅰ和Ⅱ中硒的测定方法.方法供试品经25%盐酸溶液稀释,采用流动注射氢化物发生原子吸收分光光度法测定硒含量.结果本法检出限为0.30μg·L-1,方法的线性范围为0～40μg·L-1,回收率分别为96%～99%,变异系数RSD<3%.结论该方法操作简便、快速、灵敏、单次测定样品量大,可以用于多种微量元素注射液中硒的质量控制.     

原子吸收分光光度法测定磺胺嘧啶银的含量

目的建立原子吸收分光光度法测定磺胺嘧啶银的含量方法。方法应用原子吸收分光光度法进行测定,采用标准曲线法计算样品含量。结果平均回收率为99.89%,RSD=0.21%。结论所用方法准确、精密度高,可作为该药的质量控制方法。     

Utilization of membrane filtration for preconcentration and determination of Cu(II) and Pb(II) in food,water and geological samples by atomic absorption spectrometry

A method for separation–preconcentration of Cu(II) and Pb(III) ions by membrane filtration has been presented. The analyte ions were collected on acetate membrane filter as their 1-2-pyridylazo 2-naphthol (PAN) complexes. The analytes were determined by flame atomic absorption spectrometry. The analytical parameters including pH, eluent type, sample volume, amount of PAN, etc. were examined in order to gain quantitative recoveries of analyte ions. The effects of foreign ions on the recoveries of analyte ions were also investigated. The detection limits by three sigma were found to be 1.2 and 3.5 μg L⁻¹ for Cu(II) and Pb(II), respectively. The preconcentration factor was 60 for Cu(II) and 20 for Pb(II). The validation of the presented procedure was checked by the analysis of certified reference materials. The optimized method was successfully applied to food, water and geological samples with good results.     

A novel preconcentration procedure using cloud point extraction for determination of lead,cobalt and copper in water and food samples using flame atomic absorption spectrometry

In this work, a new cloud point extraction (CPE) procedure was developed for the separation and preconcentration of lead(II), cobalt(II), and copper(II) in various water and food samples. Complexes of metal ions with 1-Phenylthiosemicarbazide (1-PTSC) were extracted into the surfactant-rich phase of octylphenoxypolyethoxyethanol (Triton X-114) from samples. After phase separation, the enriched analytes were determined by flame atomic absorption spectrometry (FAAS). Factors affecting cloud point extraction, such as pH, reagent and surfactant concentrations, temperature, and incubation time were evaluated and optimized. The interference effect of some cations and anions was also studied. After optimization of the CPE conditions, the preconcentration factor of 25 and the limits of detection (L.O.D.) obtained for lead(II), cobalt(II), and copper(II) based on three sigma (n = 20) were 3.42, 1.00, and 0.67 μg L⁻¹, respectively. The method presented precision (R.S.D.) between 1.7% and 4.8% (n = 7). The presented preconcentration procedure was applied to the determination of metal ions in reference standard materials (SRM 1515 Apple leaves and GBW 07605 Tea) and some real samples including tap water, spring water, sea water, canned fish, black tea, green tea, tomato sauce and honey.     

火焰原子吸收光谱法测定甘肃省鲜卑花属植物叶中的微量元素

目的:运用火焰原子吸收光谱法直接测定了甘南地区三个不同采集地的鲜卑花属植物叶中锌(Zn)、铜(Cu)、锰(Mn)、铁(Fe)、钴(Co)、镍(Ni)、镁(Mg)七种微量元素的含量.方法:用混合酸硝化样品,采用标准曲线法测定.结果:所测定的三个不同采集地中含有的人体必需微量元素略有差异.结论:本方法简单、准确,回收率在96.8%～102.3%之间,相对标准偏差(RSD)在0.78%～2.15%之间,结果令人满意.     

Determination of cadmium in wine by electrothermal atomic absorption spectrometry

A method is described for direct electrothermal atomic absorption spectrometric (ETAAS) determination of cadmium in untreated samples of wine. Pyrolytic graphite tubes and graphite tubes with standard L'vov pyrolytic platforms were tested as atomizers. The detection limit achieved was 0.08 microg L(-1) Cd in wine. The relative standard deviation for the concentration range from 0.2 to 10 microg L(-1) Cd ranged from 1 to 7%. The accuracy of the method was confirmed by comparing the current results with those found for wet digested wine samples and by the analysis of spiked samples. By applying the proposed method it was found that the cadmium concentration in Macedonian wines ranges from 0.10 to 0.90 microg L(-1).