892 resultados para åk 4-6
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The magnetic properties of naturally layered intermetallic compound SmMn2Si2 with textured structure have been studied. There exist a ferromagnetic transition at 35 K and two antiferromagnetic transitions at 120 and 230 K. The antiferromagnetic state below 230 K exhibits different magnetoresistance, with a negative magnetoresistance of 3%-4% for current I applied perpendicular to the c axis and with a positive magnetoresistance effect of about 4%-6% for current I parallel to the c axis. The observed magnetoresistance is likely to be related to magnetovolume effects. In the ferromagnetic state, a positive magnetoresistance with a maximum increase of 22% under an applied field of 5 T is observed at 4 K, and both H perpendicular to I and H parallel to I configurations show positive magnetoresistance. (C) 1997 American Institute of Physics.
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用 Siemens P4四圆衍射仪,测得了1,4-二丙氧基-2,3-二氰基萘的晶体结构。晶体属单斜晶系,空间群为 C2/C。晶格参数 a=14.987(3)A,b=10.527(2),c=11.755(2),β=118.98°(3),晶胞体积 V=1622.4(6)3,Z=4,Dc=1.205Kg/m~3,μ(MoK_α)=0.079mm~(-1),F(000)=624,T=293(2)K_o晶体结构应用直接法,解出最后的偏离因子 R=0.0554[1425个Ⅰ≥2σ(Ⅰ)衍射点]。结构分析表明,萘环的1,4和2,3位碳原子上的氢原子分别被丙氧基和氰基所取代,由于取代基的引入使萘环的结构有所改变。
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The photoluminescence of Ce3+, Tb3+ and Sm3+, and energy transfer from Ce3+ to Tb3+, Dy3+ and Sm3+ in Mg2Y8(SiOd(4))(6)O-2 are reported and discussed. The Ce3+ ion shows blue luminescence under UV excitation, and occupies simultaneously the 4f site and 6h site in the host lattice. The optimum concentrations for the D-5(3) and D-5(4) emissions of Tb3+ and the (4)G(5/2) emission of Sm3+ are determined to be 0.04, 0.20 and 0.10 mol in every mol of Mg2Y8(SiO4)(6)O-2, respectively. The critical distances responsible for the cross-relaxation between the D-5(3)-D-5(4) and F-7(6)-F-7(0) transitions of Tb3+ and between the (4)G(5/2)-F-4(9/2) and H-6(5/2)-F-4(9/2) transitions of Sm3+ are estimated to be 1.43 and 1.06 nm, respectively. Both Tb3+ and Dy3+ can be sensitized by Ce3+, but Ce3+ and Sm3+ quench each other.
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It is found that the nitro substituent of some aromatic bifunctional compounds shows unusual reactivity towards protonation. In the chemical ionization mass spectra of nitrobenzoic acids and their esters and amides, and of nitrophenols and their ethers, protonations on the carboxyl, ester, amide, hydroxyl or alkoxyl groups are highly suppressed by that on the nitro group. As a result, fragmentations based on protonation on these groups unexpectedly become negligible. Ortho effects were observed for all the ortho isomers where the initial protonation on the nitro group is followed by an intramolecular proton transfer reaction, which leads to the expected 'normal' fragmentations. Protonation on the nitro substituent is much more favourable in energy than on any of the other substituents. The interaction of the two substituents through the conjugating benzene ring is found to be responsible for this 'unfair' competitive protonation. The electron-attracting nitro group strongly destabilizes the MH+ ions formed through protonation on the other substituent; although the COR (R = OH, OMe, OEt, NH2) groups are also electron-withdrawing, their effects are weaker than that of NO2; thus protonation on the latter group produces more-stable MH+ ions. On the other hand, an electron-releasing group OR (R = H, Me, Et) stabilizes the nitro-protonated species; the stronger the electron-donating effect of this group the more stable the nitro-protonated ions.
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Electrochemical polymerization of 4-vinylpyridine produced a uniform poly(4-vinyl)pyridine(PVP) film on the glassy carbon (GC) electrode surface. The isopolymolybdic acid-PVP film-modified electrode was prepared by soaking the PVP/GC electrode in the 0.05 M H2SO4 aqueous solution containing 0.005 M isopolymolybdic acid (H4Mo8O26). The latter (catalyst) is incorporated and held in the PVP film electrostatically. The electrochemical behavior and electrocatalytic properties of this H4Mo8O26-PVP/GC electrode was described. The results indicate that this modified electrode has good stability and electrocatalytic activity on the reduction of chlorate and bromate ions in aqueous solution. The catalytic process is regarded as an EC mechanism.
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By doping Sb, Ba and In to the Bi-system and with the variation of nominal atomic ratio of Cu, Sr and Ca, a new possible phase is found with T(c) almost-equal-to 105 K, but with a structure of 2212 phase. Effects of post-sintering treatment from air-quenched to O2-annealed were investigated for the approximately 105 K new phase.
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本论文的研究工作由两部分组成,第一部分研究了海带(Laminaria japonica)水提取物中的活性物质,并研究了提取物对蔬菜促生长的影响及其作用机制。第二部分对三列凹顶藻(Laurencia tristicha)乙醇提取物的乙酸乙酯相进行了活性筛选和化学成分研究,并对其中分离得到的单体化合物进行了生物活性筛选。 第一部分主要以中国人工养殖的海带为原料,使用与海藻多糖生产相结合的提取技术并浓缩其中的有效成分。对浓缩提取物进行了蔬菜的农田效果实验,并对作物抗旱性能的增加、作物硝酸盐积累的减少、作物品质的改善、以及作物抵抗病毒病的能力等影响进行了作用机制方面的研究。海藻浓缩提取物进行的农田效果实验表明:作物抗旱型相对含水量RWC值在92%~94%之间;病毒病的防治效果最高可达到91%;作物的品质有明显的改善,最重要的是首次发现海藻提取物有降低蔬菜中硝酸盐的含量(硝酸盐的含量是与有机蔬菜区别的重要指标之一)的作用。该部分研究工作的创新性主要体现在:(1)首次在国内外提出和采用与海藻多糖生产相结合的提取技术。该技术的应用不但减少了提取成本,使工业化生产成为可能,更重要的是使我国的海藻工业生产可能实现高值化和开辟综合利用的新途径。(2)首次发现海藻中的小分子海藻多糖具有和细胞激动素、甜菜碱、植物生长素等活性物质同样的生物活性。 第二部分的研究是在查阅了大量的近20年来国内外有关红藻凹顶藻中化学成分研究的相关文献的基础上,对凹顶藻中的次生代谢产物进行了综述。该论文主要是通过对红藻三列凹顶藻的95%乙醇提取物的乙酸乙酯相进行化学成分分析和生物活性筛选以期能够发现具有药用前景的活性先导化合物。 为了寻找具有生物活性的化合物,我们对采自我国南海硇洲岛海域的红藻三列凹顶藻的95%乙醇提取物的乙酸乙酯相进行了活性筛选。采用MTT法对其在KB细胞株、Bel-7402细胞株、PC-3M细胞株、MCF-7细胞株、Ketr-3细胞株模型上进行了细胞毒活性测试;采用酶模型对其进行了Na+,K+-ATPase的抑制活性测试;采用MTT法对其在犬主动脉血管模型上进行了血管平滑肌细胞增殖抑制活性测试;结果表明,三列凹顶藻的95%乙醇提取物的乙酸乙酯相对Na+,K+-ATPase和犬血管平滑肌细胞增殖具有一定的抑制活性。 利用正相和反相色谱、Sephadex LH-20色谱以及反相HPLC等手段进行分离纯化,从我国南海海域的红藻三列凹顶藻中分离得到33种化学成分,通过波谱学方法(IR、MS、NMR)以及X-ray单晶衍射试验对其化学结构进行了确证,其中化合物L1~L8为新结构化合物,化合物L5为具有新骨架的全新结构化合物,化合物L9~L13为新天然产物,化合物L18和L22系首次从海洋生物中获得,所有化合物均为首次从该属海藻中得到。新化合物L1~L8均为倍半萜类化合物,命名分别为:(1R,3R)-(-)-3-(3-hydroxy-4-methylphenyl)- 1,3-dimethyl–2-methylidene cyclopentanol (L1), (1R,3R)-(-)-3-(4-methylphenyl)-1,3-dimethyl-2-methylidenecyclopentanol (L2), (1R, 3R)-(-)-3-(2-hydroxy-4-methylphenyl)-1,3-dimethyl–2–methylidenecyclopentanol (L3),(+)-(1S,2R)–2-(3–hydroxy–4–methylphenyl)-1,2-[3.1.0]bicy-clohexane (L4),()-(1S,2R) -5-hydroxy–6–methyl-spiro-dihydrobenzofuran-2(3H),2-{1-methyl-[3.1.0]bicyclohexane} (L5), (+)-6-methyl-2-(p-tolyl)hept-4-en-2,6-diol (L6),(3R,3aS,8bS)-(-)-2,3,3a,8b–tetrahydro–7-bromo – 3 a– hydroxymethyl - 3, 6, 8b - trimethyl-1H- cyclopenta[b] benzofuran (L7 ),(3R, 3aS, 8bS) - (-) - 2,3,3a,8b–tetrahydro–3 a–hydroxymethyl-3,6,8b -trimethyl -1H – cyclopenta [b] benzofuran (L8)。25个已知结构化合物确定为:(+)-(1R,2R)-4-bromo-1,5, 9–trimethyl–12– methylidene–8–oxa-tricyclo[7.2.1.02]dodeca-2,4,6-triene (L9),(3S,3aR,8bS)-(-)-2,3,3a, 8b– tetra -hydro–7-bromo–3–hydroxy-3,3a,6,8b-tetramethyl-1H-cyclopenta[b]benzofu- ran (L10 ),(3R, 3aR, 8bS) - (-) - 2, 3, 3a, 8b – tetrahydro – 7 - bromo – 3 – hydroxy - 3,3a,6,8b - tetramethyl - 1H - cyclopenta [b] benzofuran (L11 ),(3S,3aR,8bS) - (-) - 2, 3, 3a, 8b – tetrahydro –3–hydroxy -3, 3a, 6, 8b - tetramethyl-1H-cyclopenta[b]benzofuran (L12 ), ( 3aR, 8bS) - (-) - 3a,8b –dihydro–7 - bromo – 3, 3a, 6, 8b - tetramethyl - 1H - cyclopenta[b]benzofuran (L13 ),aplysinol (L14 ) ,aplysin (L15),laurebiphenyl (L16),johnstonol (L17),gossonorol (L18),7,10-epoxy-ar- bisabol-11-ol (L19),10-epi-7,10-epoxyarbisabol-11-ol (L20) 3β-hydroxy- 5α, 6α-epoxy- β- ionone (L21 ),3β-hydroxy-5β,6β-epoxy-β-ionone (L22 ),胆甾醇 (L23 ),胆甾-5-烯-3β,7α二醇胆甾-5-烯-3β,7α二醇 (L24),β-谷甾醇 (L25),叶绿醇 (L26 ),玉米黄素 (L27 ),对羟基苯甲醛 (L28 ),3-吲哚甲醛 (L29 ),1-O-十六烷酰基-3-O-β-D-吡喃半乳糖基-丙三醇(L30 ),1-O-十八烷酰基-3-O-β-D-吡喃半乳糖基-丙三醇 (L31 ),丙三醇-1-软脂酸单酯 (L32 ),正十六碳酸 (L33 )。 采用MTT法对其中23个单体化合物在Bel-7402细胞株、BGC-823细胞株、A549细胞株、A2780细胞株、HCT-8细胞株和HELL细胞株模型上进行了细胞毒活性测试;采用MTT法对其中13个单体化合物在犬主动脉血管模型上进行了血管平滑肌细胞增殖抑制活性测试;结果表明,部分单体化合物显示出一定的生物活性。
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The title coordination polymer, {[Ni3Na(OH)(C9H3O6)(2)( H2O)(11)] center dot 1.5H(2)O}(n), is built up from three independent Ni-II ions and one Na-I cation bridged by benzene-2,4,6-tricarboxylate ( BTC) ligands and water molecules. Three Ni-II ions are bridged by three bidentate carboxylate groups of three BTC ligands, two aqua ligands and one OH- unit, to form a trinuclear metal cluster. The Na-I cation is bonded to the Ni-II cluster by two bridging water molecules. One of the three BTC ligands bridges neighbouring clusters into one-dimensional chains, which are further connected through a complex hydrogen-bonding scheme, forming a three-dimensional suprastructure. The title complex is isomorphous with the previously reported Co-II complex.
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目的:建立反相高效液相色谱法同时测定四川及青海地区部分獐牙菜中獐牙菜苦苷、龙胆苦苷、芒果苷、当药醇苷、异荭草苷、1,8-二羟基-3-甲氧基(口山)酮的含量.方法:采用RP-HPLC,使用Kromasil C_(18)(4.6 mm×250mm,5 μm)柱;流动相甲醇-水(含0.02%磷酸);梯度洗脱程序为0~50 min,甲醇的体积分数(下同)由20%上升至80%;50~55 min由80%增至100%,55~60 min为100%,流速1 mL•min~(-1),检测波长254 nm;柱温35 ℃.结果:6种成分均达到基线分离,线性良好.结论:该方法快速、准确、重复性好,为该类药材的入药提供了理论依据.
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目的:对野生和栽培藏药麻花艽中龙胆苦苷、落干酸、獐牙菜苦苷和獐牙菜苷4种苦苷类成分进行高效液相色谱的含量测定,并比较分析它们之间的差异。方法:采用Eelipse XDB-C_8色潜柱(4.6 mm*150 mm,5 μm),流动相A为95%乙腈水溶液,B为5%乙腈(含10 mmol•L~(-1)的甲酸)水溶液,A在0-20min内比例由0-100%进行线性洗脱,流速1.0 mL•min~(-1),检测波长240 nm,柱温30℃。结果:4种成分均达到基线分离,龙胆菁苷、落干酸、獐牙菜苦苷、獐牙菜苷的线性范围分别为0.60~19•20μg(r=0.9999),0.24~7.68μg(r=O.9999),0.38-12.02μg(r=O.9999),0.05~1.66μg(r=0.9999);回收率分别为99.73%,98.13%,98.45%,96.22%。结论:栽培藏药麻花艽中苦苷类成分的含量已经接近或超过野生种的水平,可初步代替野生药材人药。
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对青藏高原东北部高山冰缘地区和相邻低海拔地区59种多年生草本被子植物进行了染色体计数。其中,45个种的染色体记数为首次报道,并确定其信性.对分布于高山冰缘地区和冰缘以下不同海拔地区植物染色体的多倍性进行分析研究,结果如下:(1)多年生草本被子植物多倍体频率随海拔高度上升而增加:海拔2000-3000m,多倍体频率为29.4%-47.1%.3000-3800(4000)m(高寒灌丛-草甸区),多倍体频率为33.3%-53.3%;4000-5200m以上的高山冰缘地区,多倍体频率达55.6%-70.4%.(2)高山冰缘地区新多倍体较多,并且与青藏高原上特有的植物类群(特有属、亚属或特有种)相关联。(3)分布在冰缘地区的多倍体广布种,通常都是较原始类群的古多倍体,它们可能在青藏高原强烈隆升以前就已经形成,并分化出许多生态型,在高原强烈隆升并出现高山冰缘环境以后,某些生态型突出繁殖适应机制(r型选择机制),能开拓新生境而在新出现的严酷而不稳定的冰缘地区繁衍,其它一些生态型则依靠营养生长优势(K型选择机制)广泛分布在其稳定、成熟的生境中。(4)冰缘以下地区的多倍体特有种多数属于古多倍体或次生多倍体。它们多数可能是由西南山地或秦岭、华北森林区系产生,然后扩散至青藏高原边缘。
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This paper describes the simultaneous determination of allantoin, quercetin, and 1-methyl-1,2,3,4-tetrahydro-beta-carboline-3-carboxylic acid (MTCCA) in Nitraria tangutorum Bobr seed by HPLC-APCI-MS and CE (capillary electrophoresis) methods. The final optimized chromatographic conditions were investigated in a reversed-phase Eclipse XDB-C8 column (150 x 4.6 mm, 5 mu m). A seventeen-minute gradient elution, (A: aqueous acetonitrile 20% (v/v); B: aqueous acetonitrile 60% (v/v); C: pure acetonitrile 100%) at a flow rate of 1.0 mL/min was selected for the separation of three natural products with diode array detection (DAD) at 220 nm. A CE experiment was carried out in a fused silica capillary with 32 mmol/L boric acid (pH 10), 32 mmol/L SDS and acetonitrile (10.0%, v/v). The applied potential and temperature was, respectively, set at 19 kV and 25 degrees C. After development, the validation was performed in parallel for HPLC and CE, with the same standards and sample to avoid differences due to the manipulation. The validation parameters of both techniques were adequate for the intended purpose.
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Kunyushan composite granite pluton is located in northeast part of the Sulu UHP collisional belt, Jiaodong peninsula, eastern China. It is regarded as the boundary of the Jiaodong block and the Sulu UHP collisional belt. The body is unique in the Dabieshan-Sulu UHP collisional orogen for its feature of multiple intrusions of diverse types granitoid rocks in a long span after UHP the collision between the North China and the Yangtze plates in late Triassic. It can be grouped into four series on the basis of petrology and petrochemistry. They are mid-K calc-alkaline granitoids, strongly peraluminous granites, high-K calc-alkaline granitoids and syenitic granite of shoshonitic series. In this thesis, the later three types of rocks are investigated geochronologically in detail. The grain zircon U-Pb isotope dilution dating technique has been employed in this study. Zircon morphology are presented and discussion on the chemical and physical conditions of the granite formation have been carried out in addtion. Strongly peraluminous granites comprises foliated monzogranite and garnet bearing leucogranite. They occupy more than half of the area of the Kunyushan composite body. Three zircon samples of foliated monzogranites have been analyzed, they yield lower intercept ages mainly in the range of 140-150 Ma. The formation of these rocks was likely to be at 700-600 ℃, implied by zircon morphology. Two zircon samples of the garnet bearing leucogranite yield lower intercept ages from 130 Ma to 140 Ma. Zircon morphology indicate that the liquidus temperature of the magma was about 750 °C. Syenitic granite of shoshonitic series occur in the north central part of the body, and the volume is quite small contrast to other types. One zircon sample was chosen from this rock, and yield lower intercept age of 121+1.8/-2.1 Ma. Zircon morphology indicate that the liquidus temperature of this rock is up to 900 °C, which is much higher than others'. High-K calc-alkaline granitoids can be divided into two types on the basis of rock texture and structure. One is Kf-porphyritic monzogranite. It's outcrop is quite small. Zircon ages of one sample constrain the emplacement of this rock at about 112 Ma. The other is medium-grain to coarse-grain monzogranite. Zircons from it yield lower intercept age of 100.5+2.9/-4.6 Ma. The variation of zircon morphology suggest that these two monzogranites were outcomes of a single magma at different stage. The former emplaced earlier than the latter. The liquidus temperature of the magma was about 800 ℃ Inherited zircon is ubiquitous in the Kunyushan composite body. Most of the samples yield upper intercept ages of late Proterozoic. It was considered that only the Yangtze plate underwent a crustal growth during late Proterozoic among the two plates which involved into the UHP collision. Inherited zircon of about 200 Ma can also be observed in strongly peraluminous and high-K calc-alkaline granitoids. Two samples out of eight yield upper intercept ages of Achaean.
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铊是一种有毒有害的重金属元素,已经引起了广泛的关注。本论文通过对黔西南铊矿区土壤和沉积物样品的菌株分离、铊高耐受性菌株的筛选、胞外吸附、富集、亚细胞水平区系分布、絮凝实验及ITS序列等实验研究分析,并结合铊的地球化学相关研究,较系统地阐述了真菌--铊的生物地球化学过程机理,得出以下结论: 1、与环境背景区相比,黔西南滥木厂铊矿区内的河流、土壤中铊的已有不同程度的积累,直接导致了当地微生物生物量在很大程度上的降低,微生物生物量与铊含量间有显著的负相关关系。研究区内的沉积物、土壤中的微生物区系结构和数量发生了明显变化,细菌、真菌及放线菌数量均出现显著降低,而且三大微生物对重金属污染的敏感性大小也不一样,即放线菌>细菌>真菌。从土壤样品中分离到的主要菌群仍为常见种属,如青霉属(Penicillium)、木霉属(Trichoderma)、拟青霉(Paecilomyces)等。 2、经过初筛菌株的铊耐受性实验,在1000 mg/L水平筛选得到九株高耐受性菌株。吸附实验表明:微生物菌株对铊的吸附效率在4.63~16.89%,且随着环境中铊浓度的上升而降低,这可能是因为铊浓度的升高加大了对微生物生长的抑制作用,所形成的菌丝体(或菌丝球)减少,表面积也相应减少,从而导致了吸附效率的下降。各种常量元素和铊的关系呈显著相关性,钙、钾和钠等常量元素也是微生物赖以维持生存的因子,可能由于微生物细胞对钙、钾的吸附方式与对铊的吸附方式类似。因此,随着铊处理浓度的上升,钙和钾的吸附量也随之减少,而钠则呈现相反的趋势。 3、富集实验表明,九株菌株对铊的富集量随着铊处理浓度上升而降低,其影响趋势与对生物量的影响趋势基本一致,最高可达到7189 mg/kg,最大富集系数为7.2。九株菌株对常量元素的富集与对铊的富集并无明显的相关性,但在考察铊处理浓度对常量元素的富集影响时发现,铊处理浓度的上升与对钙的富集量表现出较强的正相关;而对钾、钠、镁的富集影响并不明显。 4、亚细胞水平上的铊分布研究表明,铊的富集优先顺序为:细胞质>细胞壁>细胞器。亚细胞水平的区隔化作用是微生物对铊的主要耐受机制,细胞质是赋存铊的主要场所(53.83~79.45 %)。结合各亚细胞组分中常量元素与铊之间的相关性,并联系前人的研究,Tl+主要是通过细胞壁的Na+ -K+ ATPase和K+ -电位门通道进入细胞内的从而影响细胞的正常代谢的,而Ca2+的活化更有助于这一过程。 5、絮凝实验表明,培养三天后的发酵液对矿区废水中铊的去除率最高可达到70.49 %,最佳影响因子组合为:pH=8,温度为16℃,搅拌时间为4分钟。菌株的絮凝活性最高可达到57.32%,最佳影响因子组合为:pH=8,温度为14℃,搅拌时间为4分钟。 6、通过对九株铊高耐受性菌株的ITS序列分析及其在Gene Bank中的BLAST比对结果表明,五株菌株同属于木霉属(Trichoderma),两株菌株同属于青霉属(Penicillium)。这表明这两类真菌对铊的适应性较强,为以后寻找铊高耐受性菌株及其资源化利用提供了理论基础。
Resumo:
A new nonadentate ligand, N, N, N-1, N-1-[2,6-bis(3'-aminomethyl-1 1'-pyrazolyl)-4-phenylpyridine]tetrakis(acetic acid) (BPTA) for a Tb3+ fluorescent complex was synthesized. The Tb3+ complex is strongly fluorescent, having a large fluorescence quantum yield of 1.00 and very long fluorescence lifetime of 2.681 ms in 0.05 M berate buffer of pH 9.1. Streptavidin (SA) was labeled with SPTA by using its succinimidyl monoester, and the BPTA-Tb3+-labeled SA was used in sandwich-type time-resolved fluoroimmunoassay (TR-FIA) of alpha -fetoprotein (AFP) and carcinoembryonic antigen (CEA) in human sera. The Tb3+-labeled SA was also used in competitive type TR-FIA of bensulfuron- methyl (BSM) in water. The detection limits of these assays are 42 pg/mL for AFP, 70 pg/mL for CEA, and 0.4 ng/mL for BSM. In addition, a new simultaneous measurement method for AFP and CEA in a human serum sample was developed by using 4,4'-bis(1 " ,1 " ,1 " ,2 " ,2 " ,3 " ,3 " -heptafluoro-4 " ,6 " -hexanedion-6 " -yl)chlorosulfo-o-terphenyl ((BHHCT)-Eu3+-labeled anti-AFP antibody, biotinylated anti-CEA antibody, and BPTA-Tb3+-labeled SA. The concentrations of AFP and CEA in 39 human serum samples were determined, and the results were compared with those of the independently determined AFP and CEA by TR-FIA with a single-label method. A good correlation was obtained with the correlation coefficients of 0.991 for AFP and 0.994 for CEA.