ICP–MS法测定食品接触纸制品中铬、镍、砷、镉、铅、汞

建立电感耦合等离子体质谱法(ICP–MS)测定食品接触纸制品中铬、镍、砷、镉、铅、汞6种重金属含量的方法。样品经微波消解处理后用ICP–MS进行测定,内标法定量。在优化实验条件下,测定汞元素的线性范围在0~10μg/L之间,测定铅、镉、铬、镍、砷元素的线性范围在0~100μg/L之间,相关系数均大于0.999。各元素的检出限为0.001~0.1 mg/kg,加标回收率为89.3%~116.0%,测定结果的相对标准偏差为3.5%~7.9%(n=6)。该方法样品处理简单,检测灵敏度高,适用于食品接触纸制品中铬、镍、砷、镉、铅、汞的检测。     

微波消解-电感耦合等离子体质谱法测定砂仁中的铜、铅、砷、镉

建立了微波消解样品,电感耦合等离子体质谱法(ICP–MS)测定黔西南高砷土壤种植的砂仁中痕量铜、铅、砷、镉的分析方法。对微波消解条件进行了优化。为了避免消解试剂对质谱测定的干扰,选择硝酸–双氧水混合溶液(体积比为3∶1)作为微波消解试剂,采用ICP–MS测定消解液中铜、铅、砷、镉的含量。利用校正方程对砷、镉的质谱干扰进行校正。铜、铅、砷、镉4种元素的线性相关系数均大于0.999 2,检出限分别为0.073,0.048,0.39,0.062μg/L,测定结果的相对标准偏差小于4.5%(n=5)。各元素的加标回收率在96.0%～105.0%之间。该方法样品处理快速、简单,溶解率高,测定结果准确、可靠,适用于成批量砂仁样品中铜、铅、砷、镉微量元素的测定。     

电热板消解与密闭罐消解对土壤中49种矿质元素ICP-MS法检测的影响

分别采用电热板消解和密闭罐消解进行土壤样品前处理,根据加标回收实验和国家标准物质(GBW07403)验证实验,结果显示,使用电热板消解-ICP-MS法分析土壤中铍、锂、钒、铬、锰、钴、镍、铜、锌、镓、锗、砷、硒、锶、锆、铌、钼、钯、银、镉、铟、锡、钡、钽、钨、铼、铊、铅、铀可获得较好的准确性和精密度,而密闭消解罐消解-ICP-MS法则更适于土壤中钪、钇、镧、铈、镨、钕、钷、钐、铕、钆、铽、钬、铒、铥、镱、镥、铱、铂、金、钍的检测,各元素的检出限为0.311～94.36 ng/L,相对标准偏差为0.55%～5.03%.表明不同消解方法适于土壤中不同矿质元素的检测.应用所建立的方法,对新疆地区2个葡萄园的土壤样品中49种矿质元素进行了分析.     

电感耦合等离子体发射光谱法（ICP—AES）测定红糖中的微量元素

目的红糖人药胜过白砂糖和冰糖,其机理在哪？是糖中的桔水成分,或是红糖中的矿物质成分,值得研究。方法采用微波消解法处理样品,用电感耦合等离子体发射光谱法（ICP—AES）测定红糖中的微量元素。结果14种微量元素的检测限为1．1—7．3μg·L-1,方法准确度为96．7％-109．4％,方法精密度为0．88％-9．15％。结论微波消解样品快速、准确,用ICP—AES同时测定红糖中的镁、锌、铁、铜、铬、锰、钒、锶、镍、钴、硼、铅、镉和钛等14种微量元素,检出限低,适用于红糖微量元素的常规检测。     

密闭高压消解–ICP–AES测定进口铜精矿中铅、镉、汞、砷

采用密闭高压消解法对样品进行消解,用电感耦合等离子体发射光谱法(ICP–AES)测定进口铜精矿中的铅、镉、砷、汞有害元素。铅、镉、砷、汞的工作曲线分别在0~10,0~1,0~4,0~0.6μg/mL范围内线性良好,线性相关系数大于0.999。各元素加标回收率均为91.0%~104.7%,相对标准偏差均小于3%(n=7)。将密闭高压消解法与电热板加热法和微波消解法进行了比对分析,结果显示,密闭高压消解–ICP–AES法适合用于铜精矿样品的消解与测定。     

ICP–OES法检测玩具涂层中17种可迁移元素

建立了电感耦合等离子体发射光谱法(ICP–OES)法同时测定玩具涂层中17种可迁移元素的方法。样品经盐酸溶液提取,利用ICP–OES进行测定。砷、镉、钴、铬、镍、铅、锑、硒元素的线性范围为0.02~2 mg/L,铝、硼、钡、铜、锡、锶、锌、锰的线性范围为0.1~10 mg/L,汞的线性范围为0.02~0.5 mg/L,线性相关系数r≥0.996。方法检出限为0.000 2~0.015 9 mg/L,加标回收率为90.1%~108.1%,重复测定结果的相对标准偏差为0.23%~2.23%(n=6)。该方法简便、快速,具有较高的准确度和良好的精密度,适用于大多数玩具材料中17中可迁移元素的检测,能满足欧盟玩具安全指令的要求。     

微波消解–ICP–OES法测定陶土中铅和镉含量

建立微波消解–ICP–OES法测定陶土中铅和镉含量的方法。采用氢氟酸–硝酸作为消解液,微波消解法处理样品,消解液定容后直接进入耐氢氟酸的进样系统,用ICP–OES法测定陶土中重金属铅和镉的含量。结果表明,Pb和Cd检出限分别为0.027μg/m L和0.011μg/m L,回收率分别为90.5%~98.8%和95.0%~98.4%,测定结果相对标准偏差分别为1.38%和2.17%(n=7)。该方法具有快速、准确、灵敏度高等优点,适用于陶土中铅和镉含量的检测。     

ICP–AES法同时检测生蚝中铅、铜、镉、铬、铁含量时3种样品前处理方法比较

采用干法、湿法和微波消解法处理珠海生蚝样品,用电感耦合等离子体发射光谱仪在谱线Pb 220.3 nm,Cu 324.7 nm,Cd 228.8 nm,Cr 283.5 nm,Fe 259.9 nm下测定样品中铅、铜、镉、铬、铁5种重金属元素的含量。结果表明,珠海市4个养殖基地的生蚝重金属含量均在国标限量范围内。铅、铜、镉、铬、铁各元素线性相关系数分别为0.999 8,0.999 4,0.999 9,0.999 2,0.997 8,检出限分别为0.020,0.014,0.001,0.036,0.120 mg/kg。干法、湿法、微波消解法的加标回收率分别为72.8%~99.3%,88.0%~102.0%,89.0%~103.0%。微波消解处理样品,ICP–AES法同时测定4种样品中5种重金属的含量,其测定结果的相对标准偏差均小于17%。微波消解–ICP–AES适合生蚝中铅、铜、镉、铬、铁含量的快速测定。     

电感耦合等离子体质谱法测定土壤中有效态镉

建立电感耦合等离子体质谱(ICP–MS)仪测量土壤样品中有效态镉的方法。为了提高ICP–MS法测量的稳定性和准确度,优化样品粒度、称样量、振荡时间等条件,以二乙三胺五乙酸–三乙醇胺–氯化钙混合溶液(DTPA)为提取剂(固液比为1∶12.5),元素铑为内标,ICP–MS仪测定有效态镉的含量。有效态镉的线性范围为0～0.200 mg/L,线性相关系数为0.999 8,检出限为0.000 9mg/kg。测定结果的相对标准偏差为1.56%～3.16%(n=6)。用该法测定国家标准物质土壤中的有效态镉,测定值与标准值基本一致,相对误差为–2.92%～3.13%。该方法减少了样品的浪费,提高了工作效率,增加了测量稳定性,测定结果准确可靠,在检测大批量土壤有效态镉时更具有优越性。     

电感耦合等离子体质谱法同时测定食品中的铅、镉和总砷

建立了电感耦合等离子体质谱(ICP–MS)法同时测定食品中的铅、镉和总砷含量的分析方法。样品经消化后直接用ICP–MS分析,采用在线引入混合内标溶液校正基体干扰和仪器的信号漂移。铅、镉、总砷的质量浓度在0~50μg/L范围内与信号强度呈良好的线性,线性相关系数(r)均大于0.999 0。用该方法对标准物质进行测定,分别采用湿法、微波消解法对样品进行处理,两种前处理方式测定值无显著性差异,测定结果的相对标准偏差在0.45%~4.2%之间(n=6),检测结果均在参考值范围内。该方法可同时测定铅、镉和总砷含量,操作简便、重现性好、结果准确可靠,可以满足各种食品中铅、镉和总砷同时测定的要求。     

An evaluation of analytical techniques for determination of lead, cadmium, chromium, and mercury in food-packaging materials

Closed microwave digestion and a high-pressure asher have been evaluated for wet-oxidation and extraction of lead, cadmium, chromium, and mercury from a range of typical packaging materials used for food products. For the high-pressure asher a combination of nitric and sulfuric acids was efficient for destruction of a range of packaging materials; for polystyrene, however, nitric acid alone was more efficient. For microwave digestion, a reagent containing nitric acid, sulfuric acid, and hydrogen peroxide was used for all materials except polystyrene. Use of the high-pressure asher resulted in the highest recoveries of spiked lead (median 92%), cadmium (median 92%), chromium (median 97%), and mercury (median 83%). All samples were spiked before digestion with 40 μg L^–1 Cd, Cr, and Pb and 8 μg L^–1 Hg in solution. The use of indium as internal standard improved the accuracy of results from both ICP–MS and ICP–AES. Average recovery of the four elements from spiked packaging materials was 92 ± 14% by ICP–MS and 87 ± 15% (except for mercury) by ICP– AES. For mercury analysis by CVAAS, use of tin(II) chloride as reducing agent resulted in considerably better accuracy than use of sodium borohydride reagent.     

Immuno‐capture as ultimate sample cleanup in LC‐MS/MS determination of the early stage biomarker ProGRP

This paper presents a selective and efficient sample preparation procedure for NLLGLIEAK, signature peptide for the small cell lung cancer (SCLC) biomarker ProGRP, in human serum. The procedure is based on immuno‐capture of ProGRP in 96‐wells microtiter plates coated with the mAb E146. After immuno‐capture and thorough rinse, trypsin was added for in‐well digestion. Subsequently the signature peptide was enriched by SPE and determined by LC‐MS/MS. Various steps in the procedure were optimized to achieve a low LOD such as dilution of sample, tryptic digestion, and SPE cleanup and peptide enrichment conditions. A single quadropole MS was used during optimization of the method. A triple quadropole MS was used in the method evaluation in order to improve sensitivity. The evaluation showed good repeatability (RSD, 11.9–17.5%), accuracy (3.0–6.6%), and linearity (r² = 0.995) in the tested range (0.5–50 ng/mL). LOD and LOQ were in the pg/mL area (0.20 and 0.33 ng/mL, respectively), enabling the determination of clinically relevant concentrations. The method was applied to two patient samples and showed good agreement with an established immunological reference method. The final method was compared to a previous published LC‐MS method for the determination of ProGRP in serum based on protein precipitation and online sample cleanup. Both showed acceptable method performance, however, the immuno‐capture LC‐MS method was superior with respect to sensitivity. This illustrates the large potential of immuno‐capture sample preparation prior to LC‐MS in protein biomarker quantification.     

Highly sensitive determination of tetrabromobisphenol A and bisphenol A in environmental water samples by solid‐phase extraction and liquid chromatography‐tandem mass spectrometry

Using bamboo‐activated charcoal as SPE adsorbent, a novel SPE method was developed for the sensitive determination of tetrabromobisphenol A and bisphenol A in environmental water samples by rapid‐resolution LC‐ESI‐MS/MS. Important parameters influencing extraction efficiency, including type of eluent, eluent volume, sample pH, volume and flow rate, were investigated and optimized. Under the optimal extraction conditions (eluent: 8 mL methanol, pH: 7; flow rate: 4 mL/min; sample volume: 100 mL), low LODs (0.01–0.02 ng/mL), good repeatability (6.2–8.3%) and wide linearity range (0.10–10 ng/mL) were obtained. Satisfied results were achieved when the proposed method was applied to determine the two target compounds in real‐world environmental water samples with spiked recoveries over the range of 80.5–119.8%. All these facts indicate that trace determination of tetrabromobisphenol A and bisphenol A in real‐world environmental water samples can be realized by bamboo‐activated charcoal SPE‐rapid resolution‐LC‐ESI‐MS/MS.     

气相色谱-质谱法同时测定土壤中的4种丙烯酸酯类农药

建立快速溶剂萃取-气相色谱质谱联用法同时测定土壤中的4种丙烯酸酯类(嘧菌酯,嘧菌胺,苯氧菌胺,醚菌酯)残留量的分析方法。将随机采集到的土壤样品自然风干,粉碎过筛。称取过筛后的样品5 g,置于萃取池中,以丙酮-乙酸乙酯(体积比为1∶1)作为萃取溶剂,于加速溶剂萃取仪中进行提取,收集提取液,氮吹至近干,用丙酮定容至1 mL,以0.45μm滤膜过滤后,上GC-MS/MS仪分析,色谱峰面积外标法定量检测。4种丙烯酸酯类的质量浓度在0.05~5.0μg/mL范围内与其色谱峰面积呈良好的线性关系,检出限为0.006~0.010 mg/kg,加标回收率为91.4%~94.6%,测定结果的相对标准偏差为2.48%~4.29%(n=6)。该方法前处理简单,定性及定量结果准确,适用于土壤中丙烯酸酯类残留的监测。     

微波消解-电感耦合等离子体质谱法测定血液中30种微量元素

建立了微波消解-电感耦合等离子体质谱法定量测定血液中微量元素的方法.采用微波消解进行样品前处理,在硝酸-双氧水混合体系中消解后稀释,电感耦合等离子体质谱法(ICP-MS)测定全血中铜(Cu)、铅(Pb)、锌(Zn)、银(Ag)、钡(Ba)、锡(Sn)、镍(Ni)、钴(Co)、钒(V)、锑(Sb)、铊(Tl)、汞(Hg)、锰(Mn)、钼(Mo)、硒(Se)、铬(Cr)、镉(Cd)、钍(Th)、钛(Ti)、铝(Al)、砷(As)、铁(Fe)、钙(Ca)、镓(Ga)、锶(Sr)、锂(Li)、镁(Mg)、铍(Be)、钠(Na)和钾(K)元素的含量.对样品前处理过程和仪器工作参数进行了优化,通过内标校正法降低基体效应.结果表明,上述元素相关系数R^(2)均大于0.9998,检测精密度为0.142%~12.856%.方法简单、准确、快速,可精确测定全血中多种微量元素的含量,为全血中元素含量的测定提供了高效可靠的分析手段.     

微波消解ICP-MS测定海洋沉积物中微量元素

采用微波消解-电感耦合等离子体质谱(ICP-MS)法同时测定海洋沉积物中的Cr、Co、Ni、Cu、Zn、Cd、Pb7种微量元素。对微波消解酸体系和微波程序进行了优化,结果表明:由4 mL HNO3与2 mL HF组成的混合酸对沉积物消解效果好;阶段升温,最高温度200℃,消解30 min有着最佳的消解效果。采用本实验方法对7种不同类型的海洋沉积物标准物质进行了测定,测定结果与标准值一致。各元素的检出限在0.009~0.17 ng/g之间。该方法快速简便、准确度高,可用于海洋沉积物样品中多元素同时测定。     

Komplexe mit N,N,N′,N′-Tetrakis(2-hydroxybenzyl)ethylendiamin (H4tben). Kristallstruktur von Ti(tben)

Complexes with N,N,N′,N′-Tetrakis(2-hydroxybenzyl)ethylenediamine (H₄tben). Crystal Structure of Ti(tben) The complexes of N,N,N′,N′-tetrakis(2-hydroxybenzyl)-ethylenediamine with titanium(IV), vanadium(IV), manganese(IV), and tin(IV) were synthesized and characterized by mass spectrometry. The Mössbauer date were evaluated for the tin compound. The molecular structure of the titanium(IV) complex was determined by X-ray structural analysis, crystallographic data see “Inhaltsübersicht”.     

Analysis of vanadium-titanium ores and alloys

A new spectrophotometric method for determining titanium in vanadium-titanium ore with 2,2'-biquinoxalyl was developed. The analytical procedure to dissolve samples and separate titanium from vanadium and tin was elaborated as well. Furthermore, vanadium and iron were determined in the ore investigated.     

自动石墨消解–电感耦合等离子体质谱法同时测定左氧氟沙星胶囊中7种金属元素

建立自动石墨消解-电感耦合等离子体质谱法(ICP-MS)同时测定左氧氟沙星胶囊中铅、铬、砷、镉、锡、铝、铁7种金属元素含量的方法。以HNO3-H2O2()体积比为1∶1为消解体系,采用自动石墨消解法消解左氧氟沙星胶囊样品,消解液除酸后,用5%硝酸溶液定容至50 mL,采用电感耦合等离子体质谱法对消解液进行测定,以内标法定量。铅、铬、砷、镉、锡、铝、铁的质量浓度在0.05~20.0μg/mL范围内与质谱响应值成良好的线性关系,相关系数均大于0.998,方法检出限为0.119~1.323μg/kg。样品加标回收率为91.2%~105.5%,测定结果的相对标准偏差为1.67%~3.46%(n=6)。该方法样品前处理简单,检出限低,测定结果准确,适用于左氧氟沙星胶囊等沙星类抗生素中多种金属元素残留的测定。