碰撞/反应池—电感耦合等离子体质谱在食品分析中的研究
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摘要
微量元素是构成人体细胞或体液、维持机体特殊生理功能酶系的特定生理成分或激活剂,在人体的生命活动和生理过程中必不可少,具有明显营养作用,对于维持人体的生长发育、新陈代谢、生理生化反应、遗传以及能量转换等方面肩负着极其重要的使命,微量元素的缺乏会引起人体系统生化紊乱,导致生理功能异常,产生病理性变化和疾病。食品中含有丰富的微量元素,是人体微量元素的主要来源,不同微量元素在人体的生命活动中发挥的作用不同,所表现的生物学效应也存在较大差异,食品在生产、加工、运输、贮存、销售等环节中所引入的微量重金属元素污染对人类身心健康所构成的潜在威胁也已成为一个严重的食品安全问题,因此,食品中微量元素的检验是食品质量控制过程中的一个重要环节,建立食品中微量元素的相应分析测试技术,准确分析食品中微量元素的含量及其分布具有十分重要的意义。
电感耦合等离子体质谱(ICP-MS)法具有灵敏度高、线性范围宽、检测限低、能提供同位素比值信息并能同时进行多元素的测定等分析特性,在食品分析与检验中应用十分广泛。但由于食品组成的复杂性和种类的多样性以及在样品分解处理过程中消解试剂的使用所产生的质谱干扰仍然是ICP-MS技术获得得高精度分析结果所面临的难题。在常用的四极杆ICP-MS仪器的离子透镜和四极杆质量分析器之间加入了一个碰撞/反应池(CRC)所组成的碰撞/反应池-电感耦合等离子体质谱(CRC-ICP-MS)仪,当样品经ICP电离,通过采样锥和截取锥取样,经离子透镜聚焦后,在封闭的碰撞/反应池中与碰撞/反应气体产生碰撞/反应,使分析离子、干扰离子及其它离子碎片之间产生质量与电荷的差异从而达到校正干扰的目的。本文系统地阐述了CRC-ICP-MS法的基本理论和方法,并围绕CRC-ICP-MS法在食品科学领域中的分析应用进行了探索：
(1)研究了应用八极杆碰撞/反应池电感耦合等离子体质谱(ORS-ICP-MS)法测定坚果Li、Al、Ti、V、Cr、Mn、Fe、Co、Ni、 Cu、Zn、As、Se、Rb、Sr、Mo、Ag、Cd、Sn、Sb、Ba、Hg、Tl、Pb等24种微量元素的分析方法。以HNO3+H2O2混合体系为消解介质采用升压控制模式对样品进行微波消解后直接进行测定,利用5%甲醇在等离子体中的增敏效应改善了难电离元素质谱分析的灵敏度,获得了仪器的最佳质谱工作参数,以Sc、In、Bi混合内标溶液校正了分析过程中的基体效应,应用碰撞/反应系统和炬屏蔽系统校正了质谱工作过程中的多原子离子干扰。采用国家标准物质GBW10045验证了方法的准确性和精密度,所有待测元素的检出限在0.002-0.290μg/L之间。采用该法分别对国外5种坚果类进口食品美国榛子、巴西腰果、美国杏仁、美国开心果、巴西松子进行分析,结果表明,坚果内微量营养元素含量丰富,其中腰果和开心果中硒含量较高,对照我国坚果炒货食品国家标准GB/T22165-2008,所有坚果中的重金属元素含量处于极低水平,食用安全,具有较高的营养价值。该法可用于坚果类食品的质量评价和安全评估。
(2)对土豆样品采用HNO3+H2O2混合酸消解体系进行微波消解处理制样,用ORS-ICP-MS法同时测定土豆中Na、Mg、Al、P、 K、Ca、Cr、Mn、Fe、Co、Ni、Cu、Zn、As、Se、Pb共16种无机元素的含量。详细地研究了样品的前处理条件,采用八极杆碰撞／反应池(ORS)技术,通过选择不同的碰撞／反应模式,改变碰撞／反应气的流速,在确保方法灵敏度的情况下,有效地减少了多原子分子的重叠形成的质谱干扰。选用Rh作内标元素校正基体效应和信号漂移。该方法对16种待测元素的检出限为0.005-0.236μg/L,通过添加标准进行加标回收,所有待测元素的回收率在92.20%-109.65%之间,相对标准偏差(RSD)均小于3.18%,结果准确可靠。采用该法对来自不同产地的4个土豆样品进行分析,结果显示,土豆中无机元素的含量具有较大的地域性。土豆中含钾较高,钾是人体调节体液平衡、维持肌肉和神经的功能以及代谢所必需的主要营养元素,并具有抗癌防癌作用；土豆中P、Mg、Ca钙含量也较高,而重金属元素的含量很低,远低于我国食品国标限量规定标准,食用安全。该法可为土豆中无机元素的快速检测提供科学依据。
(3)建立了ORS-ICP-MS法测定食品添加剂甜味剂中Cr、Co、 Ni、Cu、As、Cd、Sn、Sb、Hg、Pb等10种重金属元素的含量。采用微波消解法消解样品后直接进行分析。考察了长时间质谱分析对待测元素信号强度的影响,在碰撞/反应池内分别通入高纯氦气或氢气,通过多原子离子与氦气或氢气的碰撞/反应来减少多原子离子的干扰,选用Sc、Y、In、Bi等元素为内标混合液校正基体效应和信号漂移,确定了实验的最佳测定条件。该方法对10种待测元素的检出限在0.003～0.038μg/L之间,加标回收率在93.0%～106.6%之间,相对标准偏差(RSD)≤3.4%。采用该法对木糖醇、阿斯巴甜、糖精钠、甜蜜素等4种常用非营养型甜味剂进行分析,结果表明,4种食品甜味剂中重金属元素的含量均低于10μg/g的限量标准。该方法简便、快速、准确,完全可以用于食品添加剂甜味剂质量控制和安全评价。
(4)利用带ORS和屏蔽炬系统(Shield Torch System, STS)的ICP-MS测定蜂蜜中Na、Mg、Al、K、Ca、Cr、Mn、Fe、Ni、Cu、 As、Se、Mo、Cd、Ba、Hg、Pb等多种微量元素。研究了在标准模式、He碰撞模式和H2反应模式下待测元素的背景等效浓度(background equivalent concentration,BEC)变化情况,结果显示,在碰撞/反应模式下,质谱分析过程中易干扰元素的BEC降低了1-3个数量级,有效地克服了多原子分子离子的干扰。该法灵敏度高,各元素的检出限在1.05-73.45ng/L之间；各待测元素线性关系良好,线性相关系数均大于0.9995；重现性好,各待测元素相对标准偏差(RSD)小于2.73%；准确度高,加标回收率在92.2%-106.8%之间。采用该法对市售的4个品种的蜂蜜进行分析,结果表明,18种微量元素在4种蜂蜜中的含量存在很大差异,蜂蜜中含有大量人体所必需的营养元素,而重金属元素的含量处于较低水平。蜂蜜是一种营养丰富、食用安全的天然滋养食品。
(5)研究了分别采用双聚焦电感耦合等离子体质谱(SF-ICP-MS)法和ORS-ICP-MS法测定食品膨松剂碳酸氢钠中Be、Mg、Al、Ca、 Cr、Mn、Fe、Ni、Cu、Zn、As、Cd、Hg、Pb等14种杂质元素的分析方法。样品经硝酸密闭微波溶解后,试液直接用SF-ICP-MS法和ORS-ICP-MS法测定上述微量元素。详细地研究了样品的消解方法、待测元素同位素的选择以及SF-ICP-MS法和ORS-ICP-MS法的差异。SF-ICP-MS法采用低分辨模式和中分辨模式有效地消除了多原子离子对待测元素的干扰,ORS-ICP-MS法采用氦碰撞模式和氢反应模式消除了多原子离子对待测元素的干扰。以Ge、In、Bi为内标元素可明显改善仪器分析的稳定性和精密度水平。结果表明,两种分析方法所测定的结果基本一致,ORS-ICP-MS法较SF-ICP-MS法具有更低的检出限。
Trace elements are the specific physiologic element or activator forming human cells or body fluids, to maintain the body's special physiological function of enzymes, it is essential in the life activities and physiological processes in the human body, and it plays an obviously nutritional role in the growth of the human organism, the process of metabolism, the biochemical reaction of physiology, and energy conversion. So it shoulders the important mission. The lack of trace elements will cause the biochemical disorders of human body system, lead to physiological dysfunction, and produce diseases and pathological problems. Rich trace elements in food are the main source of trace elements of human body. Because different trace elements play different roles in the life activity of human body, their biological effects are greatly different. The trace elements of heavy metal in food brought by food production, processing, delivery, storage and sales have been a latent threat to human health, which is a serious problem of food safety. Therefore, inspecting trace elements of food is an important step in the work of food quality control. For this, the contents and the distributions of the trace elements in foods must be accurately analyzed.
With its simple spectrum, extremely low detection limit, wide linearity range, fast analyzing speed and offering the ratios of isotopes, inductively coupled plasma mass spectrometry (ICP-MS) has been widely applied in food analysis. But as a result of the diversity of food species, the complexity of matrix and the spectral overlap interference, caused by the added solvents in the course of processing pre-sample, are still problems faced in ICP-MS analysis. However, the greatest difference of collision/reaction cell (CRC)-ICP-MS from the common quadrupole ICP-MS is to generate the differences of mass and electric charges among the analyzed ions, interfering ions and other fragment ions by putting a collision/reaction cell between the ion lens and the quadrupole mass analyzer when the sample is ionized by ICP and is taken with a sampling cone and an skimmer cone and then has a collision reaction/reaction with the collision/reaction gas in the sealed CRC after focusing with ion lens. Finally the corrections of interferences are achieved. The paper systematically expounds the theoretical foundation of CRC-ICP-MS method. And the analysis and application of CRC-ICP-MS method in food were explored in the following aspects:
(1) This paper describes a simple method for the determination of Li, Al, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sr, Mo, Ag, Cd, Sn, Sb, Ba, Hg, Tl and Pb in nuts by using ICP-MS with octopole reaction system(ORS). Under the boost control, the sample was directly determined in nitric acid and hydrogen peroxide medium after its microwave digestion. The enhancement effect arising in the plasma of5%methanol improved the sensitivity of ICP-MS measurement of the elements ionized difficultly and the working parameters of the instrument were optimized. In this work, matrix effects were corrected in the mixed standard solution of Sc, In and Bi, and an octopole reaction system (ORS) and shield torch system (STS) was used to eliminate the interference of polyatomic ions. The applicability of the proposed method was validated by the analysis of rice standard reference material (GBW10045). The result showed that the detection limits of the24elements are in the range of0.002～0.290μg/L. This method was sensitive, precise and applicable for the analysis of the trace elements in the five kinds of nuts such as Amercan hazelnut, almond, pistachio, and Brazilian cashew and pinenut. And the result of the analysis suggested that there were rich micro-nutrients in the nuts and more Selenium in cashew and pistachio. According to GB/T22165-2008(Chinese fried snack standard of nuts), all nuts are very low in heavy metal element, so with high edible value. The technique can be applied to the quality and safety evaluations of nuts.
(2) The sample of potato was achieved by microwave digestion in a digestion system of the mixed acid (HNO3and H2O2). And the contents of16inorganic elements (Na, Mg, Al, P, K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se and Pb) in the sample were determined by ICP-MS. The pretreatment of sample was studied in detail. With ORS, different collision/reaction modes were selected, the gas flow of collision/reaction was changed, and the sensitivity of the method was ensured. Consequently, the spectral interferences caused by the overlaps of polyatomic molecules were effectively decreased. Rh as internal standard element was used to compensate matrix effect and signal drift. Under the optimal conditions, the detection limits of the16inorganic elements are in the range of0.005～0.236μg/L. The recovery was92.20%～109.65%by adding standard recovery experiment, and the relative standard deviation (RSD) was less than3.18%for all the elements. This method turned out to be precise and reliable. Four potatoes from different places of origin were analyzed in the way, and the result showed that the contents of inorganic elements in potato are greatly regional. A potato contains rich potassium which is an essential and major nutrient of human body for regulating fluid balance and maintaining muscles, nerve functions and metabolism, and even can be of cancer prevention and resistance. Potato can be safely eaten because of its rich phosphorus, magnesium and calcium, and very few heavy metal elements which are far lower than the Chinese standard of the limited food quantity. This method provides scientific rationale for determining inorganic elements of potato.
(3) An analysis method of microwave digestion and ICP-MS with ORS were established for the determination of10heavy metal elements including Cr, Co, Ni, Cu, As, Cd, Sn, Sb, Hg and Pb in sweetener. The effect of long-time spectral analysis on the signal intensities of the determined elements was observed. Ultrapure helium and hydrogen was respectively inlet in the octopole/reaction cell system. The use of ORS can eliminate the interference of polyatomic ions dramatically. Sc, Y, In and Bi as internal standard elements were used to compensate matrix effect and signal drift. The optimum conditions for the determination was tested and discussed. Under the optimal conditions, the detection limits of the10elements was in the range of0.003～0.038μg/L, the recovery of the samples was in the range of93.0%～106.6%and the relative standard deviation(RSD)≤3.4%, which showed that the method was very precise. In the way four common non-nutritious sweeteners including xylitol, aspartame, saccharin sodium, and sodium cyclamate were analyzed. It turned out that the contents of the heavy metal elements in the four sweeteners are all less than10μg/g. The technique was simple, quick and precise, and it could be completely applied to the quality control and safety evaluation of food additive and sweetener.
(4) An analytical method for simultaneous determination of18trace elements in honey including Na, Mg, Al, K, Ca, Cr, Mn, Fe, Ni, Cu, Zn, As, Se, Mo, Cd, Ba, Hg and Pb by ORS-ICP-MS has been established. And the background equivalent concentrations (BEC) of the determined elements were respectively studied under the modes of normal, hydrogen reaction, and helium collision. It showed that under the modes of hydrogen reaction and helium collision the BECs easily interfering with elements greatly declined by one to three orders of magnitude, and the interference of polyatomic ions was eliminated effectively. The method was sensitive, accurate and reproducible with the detection limits in the range of1.05～73.45ng/L, good linear relations whose relevant coefficients are all more than0.9995, the RSDless than2.73%, and the recovery in the range of92.2%～106.8%. In this way four kinds of honey bought in the market were analyzed including osmanthus honey, medlar honey, jujube honey and acacia honey. The study proved that the contents of18trace elements in different kinds of honey were of great difference. In honey there are very few heavy metal elements but sufficient trace elements which are essential in human body. So honey is rather nutritious and safe to drink.
(5)An analytical method was examined to determine14incidental elements including Be, Mg, Al, Ca, Cr, Mn, Fe, Ni, Cu, Zn, As, Cd, Hg and Pb in sodium bicarbonate-a food bulking agent respectively by adopting sector field inductively coupled plasma mass spectrometry (SF-ICP-MS) and ORS-ICP-MS. The sample was dissolved by HNO3in a closed-vessel microwave system, and then the above14trace elements in the test solution were determined directly by SF-ICP-MS and ORS-ICP-MS. This technique covered in detail the digestion method of the sample, the selection of the isotopes of the determined elements and the differences between SF-ICP-MS and ORS-ICP-MS. SF-ICP-MS was applied to the low or middle resolution mode to eliminate the interference of polyatomic ions with the determined elements, while ORS-ICP-Ms was applied to helium collision mode and hydrogen reaction mode to eliminate the interference of polyatomic ions with the determined elements. Ge, In and Bi as internal standard elements apparently improved the stability and precision of instrumental analysis. As a result, the determinations in the two analytical methods were almost identical, and the detection limits of ORS-ICP-MS were lower than ones of SF-ICP-MS.
电感耦合等离子体质谱(ICP-MS)法具有灵敏度高、线性范围宽、检测限低、能提供同位素比值信息并能同时进行多元素的测定等分析特性,在食品分析与检验中应用十分广泛。但由于食品组成的复杂性和种类的多样性以及在样品分解处理过程中消解试剂的使用所产生的质谱干扰仍然是ICP-MS技术获得得高精度分析结果所面临的难题。在常用的四极杆ICP-MS仪器的离子透镜和四极杆质量分析器之间加入了一个碰撞/反应池(CRC)所组成的碰撞/反应池-电感耦合等离子体质谱(CRC-ICP-MS)仪,当样品经ICP电离,通过采样锥和截取锥取样,经离子透镜聚焦后,在封闭的碰撞/反应池中与碰撞/反应气体产生碰撞/反应,使分析离子、干扰离子及其它离子碎片之间产生质量与电荷的差异从而达到校正干扰的目的。本文系统地阐述了CRC-ICP-MS法的基本理论和方法,并围绕CRC-ICP-MS法在食品科学领域中的分析应用进行了探索：
(1)研究了应用八极杆碰撞/反应池电感耦合等离子体质谱(ORS-ICP-MS)法测定坚果Li、Al、Ti、V、Cr、Mn、Fe、Co、Ni、 Cu、Zn、As、Se、Rb、Sr、Mo、Ag、Cd、Sn、Sb、Ba、Hg、Tl、Pb等24种微量元素的分析方法。以HNO3+H2O2混合体系为消解介质采用升压控制模式对样品进行微波消解后直接进行测定,利用5%甲醇在等离子体中的增敏效应改善了难电离元素质谱分析的灵敏度,获得了仪器的最佳质谱工作参数,以Sc、In、Bi混合内标溶液校正了分析过程中的基体效应,应用碰撞/反应系统和炬屏蔽系统校正了质谱工作过程中的多原子离子干扰。采用国家标准物质GBW10045验证了方法的准确性和精密度,所有待测元素的检出限在0.002-0.290μg/L之间。采用该法分别对国外5种坚果类进口食品美国榛子、巴西腰果、美国杏仁、美国开心果、巴西松子进行分析,结果表明,坚果内微量营养元素含量丰富,其中腰果和开心果中硒含量较高,对照我国坚果炒货食品国家标准GB/T22165-2008,所有坚果中的重金属元素含量处于极低水平,食用安全,具有较高的营养价值。该法可用于坚果类食品的质量评价和安全评估。
(2)对土豆样品采用HNO3+H2O2混合酸消解体系进行微波消解处理制样,用ORS-ICP-MS法同时测定土豆中Na、Mg、Al、P、 K、Ca、Cr、Mn、Fe、Co、Ni、Cu、Zn、As、Se、Pb共16种无机元素的含量。详细地研究了样品的前处理条件,采用八极杆碰撞／反应池(ORS)技术,通过选择不同的碰撞／反应模式,改变碰撞／反应气的流速,在确保方法灵敏度的情况下,有效地减少了多原子分子的重叠形成的质谱干扰。选用Rh作内标元素校正基体效应和信号漂移。该方法对16种待测元素的检出限为0.005-0.236μg/L,通过添加标准进行加标回收,所有待测元素的回收率在92.20%-109.65%之间,相对标准偏差(RSD)均小于3.18%,结果准确可靠。采用该法对来自不同产地的4个土豆样品进行分析,结果显示,土豆中无机元素的含量具有较大的地域性。土豆中含钾较高,钾是人体调节体液平衡、维持肌肉和神经的功能以及代谢所必需的主要营养元素,并具有抗癌防癌作用；土豆中P、Mg、Ca钙含量也较高,而重金属元素的含量很低,远低于我国食品国标限量规定标准,食用安全。该法可为土豆中无机元素的快速检测提供科学依据。
(3)建立了ORS-ICP-MS法测定食品添加剂甜味剂中Cr、Co、 Ni、Cu、As、Cd、Sn、Sb、Hg、Pb等10种重金属元素的含量。采用微波消解法消解样品后直接进行分析。考察了长时间质谱分析对待测元素信号强度的影响,在碰撞/反应池内分别通入高纯氦气或氢气,通过多原子离子与氦气或氢气的碰撞/反应来减少多原子离子的干扰,选用Sc、Y、In、Bi等元素为内标混合液校正基体效应和信号漂移,确定了实验的最佳测定条件。该方法对10种待测元素的检出限在0.003～0.038μg/L之间,加标回收率在93.0%～106.6%之间,相对标准偏差(RSD)≤3.4%。采用该法对木糖醇、阿斯巴甜、糖精钠、甜蜜素等4种常用非营养型甜味剂进行分析,结果表明,4种食品甜味剂中重金属元素的含量均低于10μg/g的限量标准。该方法简便、快速、准确,完全可以用于食品添加剂甜味剂质量控制和安全评价。
(4)利用带ORS和屏蔽炬系统(Shield Torch System, STS)的ICP-MS测定蜂蜜中Na、Mg、Al、K、Ca、Cr、Mn、Fe、Ni、Cu、 As、Se、Mo、Cd、Ba、Hg、Pb等多种微量元素。研究了在标准模式、He碰撞模式和H2反应模式下待测元素的背景等效浓度(background equivalent concentration,BEC)变化情况,结果显示,在碰撞/反应模式下,质谱分析过程中易干扰元素的BEC降低了1-3个数量级,有效地克服了多原子分子离子的干扰。该法灵敏度高,各元素的检出限在1.05-73.45ng/L之间；各待测元素线性关系良好,线性相关系数均大于0.9995；重现性好,各待测元素相对标准偏差(RSD)小于2.73%；准确度高,加标回收率在92.2%-106.8%之间。采用该法对市售的4个品种的蜂蜜进行分析,结果表明,18种微量元素在4种蜂蜜中的含量存在很大差异,蜂蜜中含有大量人体所必需的营养元素,而重金属元素的含量处于较低水平。蜂蜜是一种营养丰富、食用安全的天然滋养食品。
(5)研究了分别采用双聚焦电感耦合等离子体质谱(SF-ICP-MS)法和ORS-ICP-MS法测定食品膨松剂碳酸氢钠中Be、Mg、Al、Ca、 Cr、Mn、Fe、Ni、Cu、Zn、As、Cd、Hg、Pb等14种杂质元素的分析方法。样品经硝酸密闭微波溶解后,试液直接用SF-ICP-MS法和ORS-ICP-MS法测定上述微量元素。详细地研究了样品的消解方法、待测元素同位素的选择以及SF-ICP-MS法和ORS-ICP-MS法的差异。SF-ICP-MS法采用低分辨模式和中分辨模式有效地消除了多原子离子对待测元素的干扰,ORS-ICP-MS法采用氦碰撞模式和氢反应模式消除了多原子离子对待测元素的干扰。以Ge、In、Bi为内标元素可明显改善仪器分析的稳定性和精密度水平。结果表明,两种分析方法所测定的结果基本一致,ORS-ICP-MS法较SF-ICP-MS法具有更低的检出限。
Trace elements are the specific physiologic element or activator forming human cells or body fluids, to maintain the body's special physiological function of enzymes, it is essential in the life activities and physiological processes in the human body, and it plays an obviously nutritional role in the growth of the human organism, the process of metabolism, the biochemical reaction of physiology, and energy conversion. So it shoulders the important mission. The lack of trace elements will cause the biochemical disorders of human body system, lead to physiological dysfunction, and produce diseases and pathological problems. Rich trace elements in food are the main source of trace elements of human body. Because different trace elements play different roles in the life activity of human body, their biological effects are greatly different. The trace elements of heavy metal in food brought by food production, processing, delivery, storage and sales have been a latent threat to human health, which is a serious problem of food safety. Therefore, inspecting trace elements of food is an important step in the work of food quality control. For this, the contents and the distributions of the trace elements in foods must be accurately analyzed.
With its simple spectrum, extremely low detection limit, wide linearity range, fast analyzing speed and offering the ratios of isotopes, inductively coupled plasma mass spectrometry (ICP-MS) has been widely applied in food analysis. But as a result of the diversity of food species, the complexity of matrix and the spectral overlap interference, caused by the added solvents in the course of processing pre-sample, are still problems faced in ICP-MS analysis. However, the greatest difference of collision/reaction cell (CRC)-ICP-MS from the common quadrupole ICP-MS is to generate the differences of mass and electric charges among the analyzed ions, interfering ions and other fragment ions by putting a collision/reaction cell between the ion lens and the quadrupole mass analyzer when the sample is ionized by ICP and is taken with a sampling cone and an skimmer cone and then has a collision reaction/reaction with the collision/reaction gas in the sealed CRC after focusing with ion lens. Finally the corrections of interferences are achieved. The paper systematically expounds the theoretical foundation of CRC-ICP-MS method. And the analysis and application of CRC-ICP-MS method in food were explored in the following aspects:
(1) This paper describes a simple method for the determination of Li, Al, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sr, Mo, Ag, Cd, Sn, Sb, Ba, Hg, Tl and Pb in nuts by using ICP-MS with octopole reaction system(ORS). Under the boost control, the sample was directly determined in nitric acid and hydrogen peroxide medium after its microwave digestion. The enhancement effect arising in the plasma of5%methanol improved the sensitivity of ICP-MS measurement of the elements ionized difficultly and the working parameters of the instrument were optimized. In this work, matrix effects were corrected in the mixed standard solution of Sc, In and Bi, and an octopole reaction system (ORS) and shield torch system (STS) was used to eliminate the interference of polyatomic ions. The applicability of the proposed method was validated by the analysis of rice standard reference material (GBW10045). The result showed that the detection limits of the24elements are in the range of0.002～0.290μg/L. This method was sensitive, precise and applicable for the analysis of the trace elements in the five kinds of nuts such as Amercan hazelnut, almond, pistachio, and Brazilian cashew and pinenut. And the result of the analysis suggested that there were rich micro-nutrients in the nuts and more Selenium in cashew and pistachio. According to GB/T22165-2008(Chinese fried snack standard of nuts), all nuts are very low in heavy metal element, so with high edible value. The technique can be applied to the quality and safety evaluations of nuts.
(2) The sample of potato was achieved by microwave digestion in a digestion system of the mixed acid (HNO3and H2O2). And the contents of16inorganic elements (Na, Mg, Al, P, K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se and Pb) in the sample were determined by ICP-MS. The pretreatment of sample was studied in detail. With ORS, different collision/reaction modes were selected, the gas flow of collision/reaction was changed, and the sensitivity of the method was ensured. Consequently, the spectral interferences caused by the overlaps of polyatomic molecules were effectively decreased. Rh as internal standard element was used to compensate matrix effect and signal drift. Under the optimal conditions, the detection limits of the16inorganic elements are in the range of0.005～0.236μg/L. The recovery was92.20%～109.65%by adding standard recovery experiment, and the relative standard deviation (RSD) was less than3.18%for all the elements. This method turned out to be precise and reliable. Four potatoes from different places of origin were analyzed in the way, and the result showed that the contents of inorganic elements in potato are greatly regional. A potato contains rich potassium which is an essential and major nutrient of human body for regulating fluid balance and maintaining muscles, nerve functions and metabolism, and even can be of cancer prevention and resistance. Potato can be safely eaten because of its rich phosphorus, magnesium and calcium, and very few heavy metal elements which are far lower than the Chinese standard of the limited food quantity. This method provides scientific rationale for determining inorganic elements of potato.
(3) An analysis method of microwave digestion and ICP-MS with ORS were established for the determination of10heavy metal elements including Cr, Co, Ni, Cu, As, Cd, Sn, Sb, Hg and Pb in sweetener. The effect of long-time spectral analysis on the signal intensities of the determined elements was observed. Ultrapure helium and hydrogen was respectively inlet in the octopole/reaction cell system. The use of ORS can eliminate the interference of polyatomic ions dramatically. Sc, Y, In and Bi as internal standard elements were used to compensate matrix effect and signal drift. The optimum conditions for the determination was tested and discussed. Under the optimal conditions, the detection limits of the10elements was in the range of0.003～0.038μg/L, the recovery of the samples was in the range of93.0%～106.6%and the relative standard deviation(RSD)≤3.4%, which showed that the method was very precise. In the way four common non-nutritious sweeteners including xylitol, aspartame, saccharin sodium, and sodium cyclamate were analyzed. It turned out that the contents of the heavy metal elements in the four sweeteners are all less than10μg/g. The technique was simple, quick and precise, and it could be completely applied to the quality control and safety evaluation of food additive and sweetener.
(4) An analytical method for simultaneous determination of18trace elements in honey including Na, Mg, Al, K, Ca, Cr, Mn, Fe, Ni, Cu, Zn, As, Se, Mo, Cd, Ba, Hg and Pb by ORS-ICP-MS has been established. And the background equivalent concentrations (BEC) of the determined elements were respectively studied under the modes of normal, hydrogen reaction, and helium collision. It showed that under the modes of hydrogen reaction and helium collision the BECs easily interfering with elements greatly declined by one to three orders of magnitude, and the interference of polyatomic ions was eliminated effectively. The method was sensitive, accurate and reproducible with the detection limits in the range of1.05～73.45ng/L, good linear relations whose relevant coefficients are all more than0.9995, the RSDless than2.73%, and the recovery in the range of92.2%～106.8%. In this way four kinds of honey bought in the market were analyzed including osmanthus honey, medlar honey, jujube honey and acacia honey. The study proved that the contents of18trace elements in different kinds of honey were of great difference. In honey there are very few heavy metal elements but sufficient trace elements which are essential in human body. So honey is rather nutritious and safe to drink.
(5)An analytical method was examined to determine14incidental elements including Be, Mg, Al, Ca, Cr, Mn, Fe, Ni, Cu, Zn, As, Cd, Hg and Pb in sodium bicarbonate-a food bulking agent respectively by adopting sector field inductively coupled plasma mass spectrometry (SF-ICP-MS) and ORS-ICP-MS. The sample was dissolved by HNO3in a closed-vessel microwave system, and then the above14trace elements in the test solution were determined directly by SF-ICP-MS and ORS-ICP-MS. This technique covered in detail the digestion method of the sample, the selection of the isotopes of the determined elements and the differences between SF-ICP-MS and ORS-ICP-MS. SF-ICP-MS was applied to the low or middle resolution mode to eliminate the interference of polyatomic ions with the determined elements, while ORS-ICP-Ms was applied to helium collision mode and hydrogen reaction mode to eliminate the interference of polyatomic ions with the determined elements. Ge, In and Bi as internal standard elements apparently improved the stability and precision of instrumental analysis. As a result, the determinations in the two analytical methods were almost identical, and the detection limits of ORS-ICP-MS were lower than ones of SF-ICP-MS.
引文
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