A new and simple microwave-assisted alkaline degradation (MAAD) method for the elimination of organochlorine-pesticide interference on the determination of polychlorinated biphenyls (PCBs) in soil by GC is presented. Under the optimal conditions, the interference of α-HCH, β-HCH, γ-HCH, δ-HCH, o.p’-DDT, p.p’-DDD and p.p’-DDT could be eliminated completely, and p.p’-DDE, Aldrin and Dieldrin could be partially eliminated; however, Dieldrin could be completely eliminated by using concentrated sulphuric acid. The method was evaluated by analyzing the spiked-soil sample. The mean recovery obtained was 84.1% and the Relative Standard Deviation (RSD) was 2.7%. Experimental results also indicate that the degradation of the interference and the extraction of the target analytes, PCBs, could be carried out simultaneously. Compared with the traditional methods, the MAAD method is a rapid, efficient and solvent-saving method.

建立了用高效液相色谱-二极管阵列法测定食品中的苏丹红含量的检测方法.本文对不同样品采用不同的前处理方法,然后用Hypersil ODS-C18色谱柱,以9:1(V/V)的乙腈-1%醋酸溶液作流动相,流速1.0ml/min,二极管阵列检测器于478nm波长下进行检测,并以保留时间和三维光谱图相似性系数进行定性.方法线性范围为0.1～50μg/ml(r=0.99986),经浓缩后样品最低检测限可达0.01mg/kg.不同样品的加标回收率为87.7%～97.7%,相对标准偏差(RSD)为2.3%～6.4%(n=6).将标准物质与样品进行同样程序的处理,可使回收率进一步提高至96%以上.此方法在测定实际样品中得到了验证.

稀土三元混配型配合物的合成实验条件苛刻,方法的重现性较差,本文合成的两种三元异配体配合物Na3[La(C7H3O6S)2(C2H5NO2)]*4H2O和[La(C6H7O7)(C2H5NO2)(NO3)2(H2O)],文献尚未见报道.近年来,人们对于稀土离子与各种类型的螯合剂及中性配体的配合倾向进行了广泛的研究.从软硬酸碱的观点看,稀土元素属于硬酸,而氧原子属于硬碱,所以稀土配合物中,含氧配体占的比例最大.各类蛋白质是生物体内各种微量元素的重要配体,而各种蛋白质[1]又是由20种天然的α-氨基酸所组成的.因此,稀土与蛋白质的相互作用可以从稀土与氨基酸配合物的研究开始,并从有关的结构数据中获得有用信息.氨基酸潜在的配位原子是羧基氧原子和氨基氮原子.用"水相直接合成法"制备的稀土氨基配合物[2],绝大多数以下列方式配位:电中性的氨基酸保留两性离子形式,通过羧基氧与稀土离子配位,而-NH+3基团不参与配位.有机羧酸[3,4]可与稀土离子生成稳定的稀土羧酸配合物.水杨酸引入磺酸基后,水溶性增大,酸性增强,能在较低的pH值与稀土生成配合物.5-磺基水杨酸以及柠檬酸与稀土形成的络合物,随酸浓度和溶液pH值的变化,配合物组成有所不同.

A sample pretreatment by microwave-assisted extraction (MAE), microwave-assisted alkaline degradation (MAAD) and microwave-assisted saponification prior to the determination of PAHs, PCBs, triazines and cholesterol in diverse samples using GC, GC-MS and HPLC has been developed. When MAAD was coupled with MAE, the degradation of chlorinated pesticides and the extraction of PCBs analytes in the samples could be carried out simultaneously. Likewise, when MAAD and MAS were coupled with MAE, the degradation, saponification and extraction could be carried out simultaneously. In addition, a microwave-assisted derivatization (MAD) of fatty acids in edible oil, plasma and shark cartilage has been developed. The analytical results are satisfactory. The microwave-assisted sample pretreatment methods are rapid, labor and solvent saving, moreover, non-chlorinated organic solvents can be used.

A rapid microwave-assisted digestion and derivatization method for the determination of fatty acids in shark cartilage by GC-MS was developed. The optimum conditions for digestion and derivatization were studied in detail using orthogonal design. The digestion and derivatization were accomplished in 4 minutes at 600 W microwave power using HCl-methanol (1:4, V/V) as digestion and derivatization solvent, and the extraction of the target analytes could be carried out simultaneously. This method is rapid, solvent-saving, and particularly suitable for the rapid determination of fatty acids in solid samples.

有机氯农药（Ops）严重干扰多氯联苯（PCBs）的测定，本文采用微波加热技术将Ops碱解，在优化的实验条件下能完全消除六六六（HCH）、双对氯苯基三氯乙烷（DDT）、二氯二苯二氯乙烷（DDD）的干扰，二氯二苯二氯乙烯（DDE）、艾试剂（Aldrin）、狄试剂（Dieldrin）也有一定数量的减少，狄试剂经浓硫酸处理后其干扰完全消除。通过对合成土壤样品的处理，表明该法能有效地碱解Ops，消除其对测定PCBs的干扰；并能在碱解Ops的同时萃取PCBs，PCBS回收率为84．1％，相对标准偏差为2．7％。本方法快速、高效，减少了有机溶剂的使用量。

A new and simple microwave-assisted alkaline degradation (MAAD) method for the elimination of organochlorine-pesticides interference on the determination of polychlorinebiphenyls (PCBs) in soil by GC is presented. Under optimized conditions, alpha-HCH, beta-HCH, gamma-HCH, delta-HCH, o, p'-DDT, p, p'-DDD and p, p'-DDT could he degraded completely, and p,p'-DDE, Aldrin and Dieldrin partly, but Dieldrin could be completely degraded by using concentrated sulphuric acid. The method was evaluated by analysing the spiked soil sample. The mean recovery obtained was 84.1% and the RSD was 2.7%. Experimental results also indicate that the degradation of the interferences and the extraction of the target analytes, PCBs could be carried out simultaneously. Compared with the traditional methods, the MAAD method is a rapid, efficient, and solvent-saving.

利用微波技术,研究了用 KOH- 甲醇、H2SO4-甲醇-甲苯、HCl-甲醇等不同体系对食用油中的脂肪酸进行衍生化,系统地比较了它们的优劣势,以及适合的分析对象.在1 min 内完成衍生化反应,选用正庚烷代替传统方法的苯+石油醚作为脂肪酸甲酯的提取剂,与传统消解及衍生化方法相比,具有节省溶剂、省时、易于操作等特点.

研究了利用微波能对样品进行加热,以H2SO4-甲苯-甲醇体系作衍生化试剂,在消化的同时对血浆中的脂肪酸进行衍生化,然后用GC-MS法测定血浆中脂肪酸.对微波功率、微波加热时间、消解及衍生化试剂等条件进行了优化,测定结果较好.该法整个消化及衍生化过程只需2min,与传统方法相比大大缩短了实验操作时间,特别适用于大量样品的测定.

采用氢化物-原子荧光光谱法测定人体血液中硒的含量.健康者(30人)血液中硒的平均含量为114.6±11.2ng·mL-1;肿瘤及心脏病患者(20人)血液中硒的平均含量为77.4±11.1ng·mL-1.研究结果表明:肿瘤及心脏病患者血液中硒的含量明显低于正常人.该方法的回收率为90.5%～107.0%,相对标准偏差为6.6%,检出极限为0.65ng·mL-1.

研究了微波消解-有机溶剂提取-气相色谱法测定鱼肉样品中有机氯农药的分析方法.对消解液、微波辅助加热条件及提取溶剂进行了优化实验,选择冰醋酸-高氯酸(体积比4:1)在600W微波功率下接受辐射2min分解鱼肉样品,用30%( )苯的石油醚溶液提取,对各种有机氯农药的回收率除p,p＇-DDT为60.3%外,其余均在83.4%～109.6%之间,与水浴加热分解的国家标准方法相当.该法具有快速,灵敏度、精确度、准确度高等优点,适用于大批量食品和生物样品中有机氯农药的分析测定.

研究了微波辅助皂化-气相色谱-质谱联用(GC-MS)测定血清中胆固醇的分析方法.用0.4 mol/L KOH-甲醇溶液为皂化液,在600 W微波功率下接受辐射30 s皂化血清样品,选正庚烷为提取液.通过与水浴皂化法、酶学分光光度法比较,表明该法快速、溶剂用量少、准确、重现性好,方法的检出限为0.011 mg,特别适用于生物、食品、体液等大量样品中胆固醇的测定,可快速为临床医学及生物工程等提供诊断数据.