电感耦合等离子体原子发射光谱法(ICP-AES)测定金鸡胶囊中的7种无机元素

建立了测定金鸡胶囊中Ca、Mg、Mn、Fe、Cu、Zn和Sr 7种无机元素含量的分析方法.采用浓硝酸和高氯酸(8+2)的混合酸溶解样品,利用电感耦合等离子体原子发射光谱法(ICP-AES)对各种元素进行测定.金鸡胶囊含有丰富的对人体有益的无机元素,对待测样品的测定结果表明,Ca、Mg、Fe、Mn、Zn、Sr和Cu的含量...     

高效液相色谱-电感耦合等离子体质谱测定蟾酥中铜、砷、镉、汞、铅含量及砷化学形态

建立了微波消解-电感耦合等离子体质谱(ICP-MS)测定蟾酥中Cu、As、Cd、Hg、Pb等元素含量的分析方法,检出限为0.28～5.7 μg/L,元素加标回收率均在91.5%～115%.用1.2 mol/L HCl浸提蟾酥中的As形态,利用高效液相色谱(HPLC)与电感耦合等离子体质谱(ICP-MS)联用技术对蟾酥样品中的As化学形态进行了初步探讨,发现其中As主要以有毒的无机As(Ⅴ)形态存在,并讨论了形态分析的方法及结果.本方法适用于蟾酥中药样品质量控制和安全评估的要求.     

离子交换色谱-电感耦合等离子体质谱法测定高纯钛中痕量杂质元素

建立了离子交换色谱-电感耦合等离子体质谱(ICP-MS)测定高纯钛中Mg、Cr、Fe、V、Mn、Co、Ni、Cu、Zn、Sr、Cd、Ba、Tl、Pb等痕量杂质元素分析方法,并对ICP-MS工作参数及条件进行了优化和选择.高纯钛用HF和HNO3溶解后进入离子色谱的阳离子交换柱,经HF(3+97)淋洗后,用HNO3洗脱,洗脱下来的溶液进入电感耦合等离子体质谱检测.方法的检出限在0.00099～0.85 μg/L之间,测定下限为0.0033～2.8 μg/L,各元素的回收率在90%～110%之间.利用本方法对纯度＞99.99%高纯钛样品的杂质元素进行分析,结果表明,其精密度和准确度均满足痕量分析的要求.     

ICP-MS法分析白花蛇舌草中16种无机元素初级形态

应用电感耦合等离子体质谱技术(ICP-MS),分析了白花蛇舌中16种无机元素的初级形态;并研究了微波辅助萃取、超声辅助萃取、恒温水浴萃取三种萃取方式对其溶出特性的影响。结果显示:白花蛇舌草中含有丰富的无机元素,这可能促进其有效成分作用的发挥。除Cu、Se外,其它元素的微波萃取的萃取效率最高;Mg、K、Ca、Mn、Ni、Se、Ba的溶解态含量较高,其他元素主要以悬浮态的形式存在于溶液中。     

有机溶剂溶样-电感耦合等离子体质谱法直接测定六氟磷酸锂中26种杂质元素

建立了电感耦合等离子体质谱(ICP-MS)法直接测定六氟磷酸锂中26种杂质元素(Be,Na,Mg,Al,K,Ca,Ti,V,Cr,Mn,Fe,Co,Ni,Cu,Zn,Ga,Sr,Zr,Mo,Pd,Ag,Cd,Sn,Sb,Ba,Pb)的分析方法。样品用无水乙醇溶解后直接用ICP-MS测定。通过在等离子体中引入氧气,避免样品溶液中高浓度碳冷凝沉积在质谱锥接口和离子透镜上导致分析元素灵敏度的降低的现象,采用碰撞/反应池(CRC)技术校正了多原子离子质谱干扰,选择基体匹配法校正了基本效应。结果表明,26种杂质元素定量标准曲线的线性相关系数不小于0.9995,检出限在0.6~31.9 ng/L之间,RSD为2.5%~7.3%,加标回收率在90.6%~108.6%之间。本方法能满足六氟磷酸锂中杂质元素的分析要求。     

高效液相色谱与电感耦合等离子体质谱联用技术用于胁迫富硒海带硒形态研究

通过对海带胁迫富硒培养, 研究了海带对硒的富集总量及硒化学形态转变. 建立了反相离子对缓冲盐等3个色谱系统的高效液相色谱与电感耦合等离子体质谱联用(RP-HPLC-ICP-MS)技术测定亚硒酸钠、硒甲基半胱氨酸(MeSeCys)、硒代蛋氨酸(SeMet)三种硒形态. 采用3种提取溶剂, 超声提取缩短提取时间, 分离检测富硒海带的主要硒形态为亚硒酸钠、硒甲基半胱氨酸和硒代蛋氨酸.     

电感耦合等离子体质谱法测定土壤中有效态微量元素

以NaNO3为提取剂,采用电感耦合等离子体质谱(ICP-MS)技术同时测定土壤中有效态Cu、Cd、Cr、Zn、Ni、Pb、Mn 7种微量元素.考察了基体效应以及质谱干扰等因素,引入Rh为内标元素有效地克服了基体效应所引起的测量偏差.方法的检出限为0.033～0.21 μg/L,样品加标回收率为92.1％～116.8％,相对标准偏差(RSD)小于6.07％.     

浒苔中有毒有害元素及砷化学形态的研究

建立了微波消解-电感耦合等离子体质谱(ICP-MS)法测定浒苔中Cu、As、Cd、Hg、Pb等元素含量的分析方法,对各元素的线性关系良好(r=0.999 3～0.999 9),检出限为0.28～2.3 μg/L,元素加标回收率为83%～108%,符合痕量分析要求.并利用高效液相色谱(HPLC)与电感耦合等离子体质谱(ICP-MS)联用技术对浒苔样品中的砷化学形态进行了初步探讨,发现其中砷主要以无机As(Ⅴ)和某种未知的砷形态存在,推测该未知砷形态为砷糖类物质.     

毛细管电泳-电感耦合等离子体质谱在痕量元素形态分析中的应用

叙述了元素形态分析的目的和意义以及发展概况，并在此基础上着重叙述了近年来毛细管电泳(CE)与电感耦合等离子体质谱(ICP-MS)联用技术在痕量元素形态分析上的应用，包括该联用技术的关键CE与ICP-MS接口的不同设计，影响CE分离分辨率及分析灵敏度的主要因素。对这种分析技术在元素形态分析上应用的潜力和限制以及发展趋势作了讨论。     

高效液相色谱-电感耦合等离子体质谱联用技术用于环境中元素形态分析的最新进展

综述了高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)联用技术在环境科学中的应用情况.参考过去十年内的国内外文献,从方法学的角度论述了HPLC联用ICP-MS技术的发展,重点探讨了该技术在环境领域,尤其是在元素形态分析(包括生物学,生物无机化学和生物医学)中的应用.     

An evaluation of extraction techniques for arsenic species from freeze-dried apple samples

The extraction of arsenic from freeze-dried apples and subsequent determination of individual arsenic species by HPLC-ICP-MS is described. Solvent extraction with sonication using various aqueous and aqueous/solvent mixtures was initially evaluated by measuring total arsenic extracted by ICP-MS. A two step procedure using overnight treatment with alpha-amylase enzyme followed by sonication for 6 h with 40:60 acetonitrile-water was found to provide good extraction efficiency. The concentration of arsenic extracted was compared with the concentration of total arsenic in the samples determined using ICP-MS after microwave digestion in order to calculate extraction efficiency. Individual arsenic species in the extracts were measured using HPLC-ICP-MS. The three most abundant arsenic species found were arsenite, arsenate and dimethylarsinic acid. Total arsenic concentrations in the freeze-dried apple samples ranged from 8.2 to 80.9 micrograms kg-1 As, dry mass. By HPLC-ICP-MS, the relative amount of inorganic arsenic in the samples ranged from 73 to 90% of the sum of the arsenic species detected in each sample.     

The extraction and speciation of arsenic in rice flour by HPLC-ICP-MS

Several solvent mixtures and techniques for the extraction of arsenic (As) species from rice flour samples prior to their analysis by HPLC-ICP-MS were investigated. Microwave-assisted extraction using water at 80 °C for 30 min provided the highest extraction efficiency. Total recoveries of extracted As species were in good agreement with the total As concentrations determined by ICP-MS after microwave-assisted acid digestion of the samples. Arsenite [As(III)], arsenate [As(V)] and dimethylarsinic acid (DMAA) were the main species detected in rice flour samples.     

胶束电动毛细管色谱法同时测定西洋参中人参皂苷Rg1、Re和Rb1

建立了西洋参中人参皂苷Rg1、Re及Rb1同时分离测定的胶束电动毛细管色谱新方法,以解决西洋参样品中难溶于水的3种人参皂苷的准确定量问题。以40.2 cm(有效长度30 cm)×50 μm的熔融石英毛细管柱为分离柱,分离缓冲液的组成为V(15 mmol/L Na2B4O7+30 mmol/L H3BO3 (pH 9.0)+100 mmol/L十二烷基硫酸钠(SDS)+30 g/L聚乙二醇35000):V(甲醇):V(异丙醇)=2:1:1,于214 nm下检测。详细研究了影响分离的因素。Rg1、Re及Rb1检出限(信噪比(S/N)为3)分别为30、40及30 mg/L,定量限(S/N=9)分别为90、120及90 mg/L,加标回收率为87.4%～95.2%。用该法测定了西洋参标准物质,并与高效液相色谱法的检测结果进行了比对,结果吻合。应用该方法分别测定了中国、加拿大及美国的西洋参,获得满意的结果。     

高效液相色谱-电感耦合等离子体质谱联用检测食品中的五种硒形态

建立了高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)联用检测硒酸盐(SeVI)、亚硒酸盐(SeIV)、硒代蛋氨酸(SeMet)、硒代胱氨酸(SeCys2)和硒代乙硫氨酸(SeEt)的方法。采用Hamilton PRP X-100色谱柱（250 mm×4.6 mm, 5 μm）,使用5 mmol/L的柠檬酸溶液(pH 4.5)作为流动相,电感耦合等离子体质谱(ICP-MS)检测,在21 min内可以完全分离5种硒形态。各形态硒的线性相关系数均大于0.9995, SeVI、SeIV、SeMet、SeCys2、SeEt的检出限分别为0.4、0.4、5.6、0.9、1.2 μg/L。探讨了不同提取方法的提取效果,鲜蘑菇和猪肉样品加标回收实验表明,对水溶性良好的无机硒和硒代蛋氨酸而言,采用柠檬酸溶液提取的效果非常好,SeIV和SeVI的回收率均在100%左右,SeMet的回收率为85.0%～95.3%;用蛋白酶水解提取,SeCys2和SeEt的回收率为79.9%～91.5%。该方法可完全满足食品中这5种硒形态的准确定量分析。     

国产西洋参花蕾中挥发油的分离与鉴定

采用气相色谱－质谱－计算机联用方法分析了国产西洋参花蕾挥发油中的化学成分,鉴定了39个化合物,其中倍半萜类总含量占52．78％,令人惊奇的是β-金合欢烯独自占了总挥发油的48．675,经与文献中测得不同部位的西洋参及同科属植物人参中的挥发油成分作对照分析,发现都共同的含有唯一相同又恰是所有测定中相对含量最高的β-金合欢烯,这一结果为阐述人参皂苷的生源合成途径提供了科学依据。     

Comparison of extraction procedures for the determination of arsenic and other elements in lobster tissue by inductively coupled plasma mass spectrometry

A variety of extraction procedures were evaluated for the extraction of arsenic and other analytes from lobster tissue samples using inductively coupled plasma mass spectrometry (ICP-MS) detection. Soxhlet, room temperature mixing, sonication, microwave assisted, supercritical carbon dioxide and subcritical water extractions were evaluated for a variety of solvent systems and optimum conditions determined using a partially defatted Lobster Hepatopancreas marine certified reference material, TORT-2 (National Research Council of Canada). The solubility trends and solvents into which the analytes extracted gave an indication as to the polar/non-polar nature of the compounds present. Analytes that prefer water are probably more polar or inorganic, while those preferring methanol solutions are less polar or organic in nature. Arsenic, cadmium, cobalt, molybdenum and selenium were probably all present in TORT-2 in both polar inorganic and non-polar organic forms. While TORT-2 may have contained similar amounts of selenium in both forms, the results suggested that more of the arsenic was present as less polar or more organic compounds, and cobalt existed mainly as more polar or inorganic species. Most of the extraction techniques suggested that, although there may be some less polar organic forms present, more of the cadmium was probably present as polar inorganic compounds. Additionally, most techniques indicated that molybdenum was possibly all less polar or more organic in nature. In general, microwave assisted extraction (MAE) yielded comparable or improved recoveries for all of the analytes monitored and usually required less solvent. Additionally, MAE proved to be the mildest, fastest, least complicated and most reproducible extraction technique evaluated. MAE at 75 degrees C for 2 min exposure time yielded quantitative recovery of arsenic from TORT-2. These conditions were evaluated for lobster tissue samples purchased from a local restaurant. Separate evaluation of the lobster meat and organs resulted in quantitative recoveries of arsenic from both tissue samples. The results indicated that the extraction efficiencies might have some dependence upon the extraction technique, extraction conditions, analyte, solvent, and sample matrix.     

Alcohol and metal determination in alcoholic beverages through high-temperature liquid-chromatography coupled to an inductively coupled plasma atomic emission spectrometer

In the present work, an inductively coupled plasma atomic emission spectrometry (ICP-AES) system was used as a high temperature liquid chromatography (HTLC) detector for the determination of alcohols and metals in beverages. For the sake of comparison, a refractive index (RI) detector was also employed for the first time to detect alcohols with HTLC. The organic compounds studied were methanol, ethanol, propan-1-ol and butan-1-ol (in the 10-125 mg/L concentration range) and the elements tested were magnesium, aluminum, copper, manganese and barium at concentrations included between roughly 0.01 and 80 mg/L. Column heating temperatures ranged from 80 to 175 °C and the optimum ones in terms of peak resolution, sensitivity and column lifetime were 125 and 100 °C for the HTLC-RI and HTLC-ICP-AES couplings, respectively. The HTLC-ICP-AES interface design (i.e., spray chamber design and nebulizer type used) was studied and it was found that a single pass spray chamber provided about 2 times higher sensitivities than a cyclonic conventional design. Comparatively speaking, limits of detection for alcohols were of the same order for the two evaluated detection systems (from 5 to 25 mg/L). In contrast, unlike RI, ICP-AES provided information about the content of both organic and inorganic species. Furthermore, temperature programming was applied to shorten the analysis time and it was verified that ICP-AES was less sensitive to temperature changes and modifications in the analyte chemical nature than the RI detector. Both detectors were successfully applied to the determination of short chain alcohols in several beverages such as muscatel, pacharan, punch, vermouth and two different brands of whiskeys (from 10 to 40 g of ethanol/100 g of sample). The results of the inorganic elements studied by HTLC-ICP-AES were compared with those obtained using inductively coupled plasma mass spectrometry (ICP-MS) obtaining good agreement between them. Recoveries found for spiked samples were close to 100% for both, inorganic elements (with both HLTC-ICP-AES and ICP-MS) and alcohols (with both HTLC-ICP-AES and HTLC-RI hyphenations).     

Ultrasonic nebulization extraction coupled with headspace hollow fiber microextraction of pesticides from root of Panax ginseng C.A. Mey

The ultrasonic nebulization extraction coupled with headspace hollow fiber microextraction (UNE-HS-HFME) was applied for the extraction of pesticides from root of Panax ginseng C.A. Mey. Experimental parameters, which affect the performances of ultrasonic nebulization extraction coupled with headspace hollow fiber microextraction, such as the kind of acceptor solvent in the pore of the fiber wall, the sample amount, extraction time, salt concentration in extraction solvent, pH of the acceptor solution, the elution time, and times were studied and optimized. The analytes were determined by high-performance liquid chromatography. The detection limits for simeton, monolinuron, chlortoluron, karmex, and prebane are 20.9, 18.4, 18.2, 12.4, and 22.2 μg/kg, respectively. Besides volatile and semi-volatile compounds, the non-volatile compounds also can be determined by the proposed method. The extraction and enrichment process can be performed simultaneously.     

Method optimization and quality assurance in speciation analysis using high performance liquid chromatography with detection by inductively coupled plasma mass spectrometry

Achievement of optimum selectivity, sensitivity and robustness in speciation analysis using high performance liquid chromatography (HPLC) with inductively coupled mass spectrometry (ICP-MS) detection requires that each instrumental component is selected and optimized with a view to the ideal operating characteristics of the entire hyphenated system. An isocratic HPLC system, which employs an aqueous mobile phase with organic buffer constituents, is well suited for introduction into the ICP-MS because of the stability of the detector response and high degree of analyte sensitivity attained. Anion and cation exchange HPLC systems, which meet these requirements, were used for the seperation of selenium and arsenic species in crude extracts of biological samples. Furthermore, the signal-to-noise ratios obtained for these incompletely ionized elements in the argon ICP were further enhanced by a factor of four by continously introducing carbon as methanol via the mobile phase into the ICP. Sources of error in the HPLC system (column overload), in the sample introduction system (memory by organic solvents) and in the ICP-MS (spectroscopic interferences) and their prevention are also discussed. The optimized anion and cation exchange HPLC-ICP-MS systems were used for arsenic speciation in contaminated ground water and in an in-house shrimp reference sample. For the purpose of verification, HPLC coupled with tandem mass spectrometry with electrospray ionization was additionally used for arsenic speciation in the shrimp sample. With this analytical technique the HPLC retention time in combination with mass analysis of the molecular ions and their collision-induced fragments provide almost conclusive evidence of the identity of the analyte species. The speciation methods are validated by establishing a mass balance of the analytes in each fraction of the extraction procedure, by recovery of spikes and by employing and comparing independent techniques. The urgent need for reference materials certified for elemental species is stressed.     

微波辅助-顶空液相微萃取/高效液相色谱分析水样中的邻硝基苯酚

建立了基于微波辅助-顶空液相微萃取在线联用、高效液相色谱法测定水样中邻硝基苯酚的分析方法。采用L16(45)正交实验设计对影响萃取的各种因素,如萃取有机溶剂、微波辐射功率、萃取时间、离子强度、样品液体积,进行了优化。优化后萃取条件为,以乙酸丁酯作为萃取溶剂,功率和时间分别为100W和12min条件下,离子强度为0的样品溶液体积为20mL。在优化萃取条件下,邻硝基苯酚的检出限LOD(S/N=3)为0.94μg/L,萃取富集倍数为30,实际水样的加标回收率为85.2%。理论分析和实验结果表明,微波辅助-顶空液相微萃取在线联用方法具有简便、快速、高效、节省溶剂、选择性好、应用范围广的特点。