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在5 % OV7/Chromosorb WAW DMCS的色谱柱上分离和测定水田除草剂2(2萘氧基) 丙酰替苯胺( 俗称萘丙胺) 。以苯二甲酸二异辛酯为内标物时,萘丙胺与内标物等之间均获得较好的分离。而且,萘丙胺的相对质量校正因子相当稳定,fW.A=0 .978 ±0.005(α= 0.05,n= 6) 。该方法具有操作简便、快速、准确度和精密度较好,对同一试样的多次平行独立测定其标准偏差≤0.90,变异系数≤1 .18 % 。该方法完全适合于水田除草剂萘丙胺的生产控制分析和产品质量的检验。 相似文献
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以R-(+)-Pulegone为起始原始经1,4-加成、溴代、水解、氧化等9步反应合成了手性辅助试剂(+)-1S,2R,5S-8-β-萘基薄荷醇及其关向异构体(-)-1R,2R,5S-8-β萘基新薄荷醇,总收率分别为24.0%和22.6%。 相似文献
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萘普生和萘普生乙酯在环糊精手性柱上的HPLC分析 总被引:2,自引:0,他引:2
以5~8μm堆积硅珠为担体,制备环糊精(β-CD)手性固定相,用此手性固定相作填料,制备手性柱;选用二氯甲烷/环己烷作洗脱液,研究不同组成的洗脱液对萘普生的光学异构体拆分效果的影响,发现洗脱液组成为:二氯甲烷+环己烷(3+7)时拆分效果较好;以上述组成的二元洗脱液,完全拆分了萘普生乙酯的光学异构体。 相似文献
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报道了以WatersBondapak^TM,ODS-C18为色谱柱,甲醇:四氢呋喃:水(72:6:22,V/V)为流动相,在UV254nm为测定波长的条件下,利用外标法定量,建立了反相高效液相色谱法测定光诱导反应粗产物中N-(α-萘基)咔唑和N-(β-萘基)咔唑的方法,为光诱导自由基链式亲核取代反应(SRN1)反应机理的探讨提供了可靠的理论依据。 相似文献
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乙烯/顺丁烯二酸酐共聚物为主链的光致变色苯氧基萘并萘醌聚合物 总被引:5,自引:0,他引:5
通过由3-溴丙-1-醇(1)与6-[4-(2-(4-羟基苯基)异丙基)苯氧基]-5,12-萘并萘醌(2)反应制备新反应试剂6-[4-(2-(4-(3-羟基丙氧基)苯基)异丙基)苯氧基]-5,12-萘并萘醌(3),然后通过(3)与乙烯-顺丁烯二酸酐交替共聚物反应的方法成功合成了乙烯-顺丁烯二酸酐为主链的光致变色苯氧基萘并萘醌聚合物(4)。与化合物(2)相似,聚合物(4)具有正常的光致变色行为。同时发现,溶剂对聚合物(4)和化合物(2)的光诱导trans→ana异构化反应速度有明显影响。在THF/H2SO4(V/V=24/1)中的速度常数约为在DMSO/H2SO4(V/V=24/1)中的速度常数的两倍 相似文献
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本文报道了以2-(6-甲基-2-苯并噻唑偶氮)-5-二乙氨基酚(MBTAE)作柱前衍生化试剂,在SpherisorbC_8柱上,以甲醇:水=80:20(V/V),含2mmol/LLi_2SO_4和10mmol/LpH5.0醋酸盐缓冲溶液作流动相,反相高效液相色谱分离和测定了Fe ̄(2+)、Co ̄(2+)、Ni ̄(2+)和Cu ̄(2+)。各金属离子的检出限(S/N=3)分别为(pg):Fe ̄(2+)6.40,Co ̄(2-)1.38,Ni ̄(2+)4.47,Cu ̄(2+)7.28。方法用于欧洲标准局,黑麦草标样的分析,所得结果与标准值相符。 相似文献
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1-(2-噻唑偶氮)-2-萘酚螯合物反相高效液相色谱法分离测定铜(Ⅱ)、铁(Ⅱ)和镍(Ⅱ) 总被引:1,自引:0,他引:1
以1-(2-噻唑偶氮)-2-萘酚(TAN)作柱前显色剂,于ODS柱上,用内含0.1mol/LLiCl,5×10-6mol/L TAN和HAc-NH4Ac缓冲溶液(pH 5.5)的甲醇-水溶液(80:20,V/V)作流动相,流速为0.6mL/min,并以紫外-可见检测器于590nm处进行检测,发展了一种RP-HPLC法同时分离测定铜(Ⅱ)、铁(Ⅱ)、镍(Ⅱ)的方法,方法灵敏度高,对于铜、铁、镍的检测限分别为1μg/L, 2 μg/L和 0.4 μg/L。用于实际样品测定,结果满意。 相似文献
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Chiral separation of racemic mixtures is of the greatest importance to the pharmaceutical industry, as the isomers of a given racemate may exhibit substantially different pharmacological effects, not to mention possibly differing toxicity behaviour. A novel chiral separation method is developed for the determination of 1-(1,4-benzodioxane-2-formyl)piperazine (BFP) enantiomers. The indirect resolution is performed by applying precolumn derivatization with the chiral reagent 2,3,4,6-tetra-O-acetyl-beta-D-glucopyranosyl isothiocyanate (GITC). The resulting diastereoisomers are separated on a reversed-phase ODS column with methanol-potassium dihydrogen phosphate (0.02mol/L, 50:50) as mobile phase. UV detection is at 250 nm. The effect of mobile phase composition upon resolution and analysis time is investigated. Two diastereoisomers show nearly base-line separation under optimal chromatographic conditions. The presented study provides a simple and accurate method for the enantiomeric quality control and the optical purity assay of BFP. 相似文献
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采用反相离子对高效液相色谱法分离测定了金属配合物{Fe[3-(2-吡啶基)-5,6-二苯基-1,2,4-三嗪]3}2+ ([Fe(PDT)3]2+)的两种几何异构体,研究了流动相中有机改性剂(乙腈、甲醇)的含量、不同种类和浓度的离子对试剂(高氯酸钠和十二烷基硫酸钠(SDS))对色谱分离的影响。并在不同的试验条件下,对所获得的色谱参数(保留因子(k)、分离度、选择性因子等)进行了探讨。在不同种类及浓度的离子对试剂条件下,二元流动相中乙腈的含量与两种几何异构体的ln k之间均呈显著的线性关系。研究进一步发现SDS的浓度变化对异构体的保留因子影响程度更为显著。在上述实验的基础上,引入更能灵活调节洗脱强度和分离度的三元流动相(乙腈/甲醇/水),优化选择了三元流动相中有机改性剂的比例以及离子对试剂的种类和浓度,使得异构体的色谱分离得到了满意的结果。实验结果表明,异构体的峰面积(A)和浓度(C)之间的线性关系良好,面式和经式异构体的检测限分别为4.28和3.44 ng/mL (S/N=3)。 相似文献
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3′,5′反向寡核苷酸是碱基组成和长度完全相同、碱基顺序相反的两个寡核苷酸序列。以三乙胺为离子对试剂,研究了缓冲液浓度(0.025~0.15 mol/L)、pH (5.0~6.8)、柱温(25~45 ℃)、流速(0.3~0.7 mL/min)以及不同初始洗脱强度和洗脱梯度条件下,6个3′,5′反向寡核苷酸模拟样品保留和分离的变化特点。三组反向序列在缓冲液浓度为0.05 mol/L,pH 6.8和流速0.4 mL/min条件下获得最大分离,温度对分离的影响不大,而初始洗脱强度对反向序列的影响远大于洗脱梯度。实验结果表明3′,5′反向寡核苷酸的分离和保留趋势不完全一致,色谱条件的优化应有利于实现样品在柱上的弱保留。研究结果还显示寡核苷酸序列中5′末端的保留强于3′末端。 相似文献
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Cyclodextrin-modified monolithic columns for resolving dansyl amino acid enantiomers and positional isomers by capillary electrochromatography 总被引:1,自引:0,他引:1
We describe beta- and gamma-cyclodextrins (beta- and gamma-CD)-modified monolithic columns prepared by sol-gel process and chemical modifications. The monolithic silica column was fabricated inside a fused-silica capillary with 100 microm inner diameter by sol-gel process. The monolithic silica matrix was chemically modified chiral selectors of beta- or gamma-CDs with a spacer of 3-glycidoxypropyltrimethoxysilane by on-column reactions. Gamma-CD-modified monolithic column has successfully been applied for the separation of dansyl amino acid enantiomers. Beta-CD-modified monolithic column has been used for the separation of the positional isomers of o-, m-, and p-cresols and the enantioseparation of racemates of benzoin and several dansyl amino acids by capillary electrochromatography, respectively. For the separation of neutral positional isomers, a positive electric field was applied. However, for the separation of negatively charged analytes, a negative electric field was applied at the inlet of column. The separation efficiency of 5.0 x 10(4) theoretical plates/m for dansyl-L-threonine was obtained at electric field strength of -300 V/cm in the mobile phase of 50 mM 2-(N-morpholino)ethanesulfonic acid (MES)-Tris/methanol (70/30) buffer at pH 7.0. L-enantiomers were eluted as the first peak. Scanning electron micrograph showed that monolithic columns have the morphology of continuous skeleton and large through-pores. 相似文献
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3′,5′反向寡核苷酸是碱基组成和长度完全相同、碱基顺序相反的两个寡核苷酸序列。以三乙胺为离子对试剂,研究了缓冲液浓度(0.025~0.15 mol/L)、pH (5.0~6.8)、柱温(25~45 ℃)、流速(0.3~0.7 mL/min)以及不同初始洗脱强度和洗脱梯度条件下,6个3′,5′反向寡核苷酸模拟样品保留和分离的变化特点。三组反向序列在缓冲液浓度为0.05 mol/L,pH 6.8和流速0.4 mL/min条件下获得最大分离,温度对分离的影响不大,而初始洗脱强度对反向序列的影响远大于洗脱梯度。实验结果表明3′,5′反向寡核苷酸的分离和保留趋势不完全一致,色谱条件的优化应有利于实现样品在柱上的弱保留。研究结果还显示寡核苷酸序列中5′末端的保留强于3′末端。 相似文献
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The enantiomeric resolution of N-t-butyloxycarbonyl (N-t-Boc) amino acids D/L isomers by reversed-phase HPLC was investigated using cyclodextrins (CD's) as chiral selectors for the mobile phase. The use of a low pH (pH<4) for the mobile phase enabled the enantioseparation of N-t-Boc amino acids. The opposite elution order of D/L isomers was observed when hydroxypropyl-derivatized beta-CD was used instead of native beta-CD. A computer simulation of the enantioseparation showed that the ratio of the retention factors of the chiral selector and the sample determined the elution order and the resolution. When the retention factor of the chiral selector is smaller than that of the sample, an isomer having larger complex formation constant eluted faster. However, when the chiral selector had a larger retention factor than the sample, an opposite elution order of the isomers was obtained. The large difference in the retention factors between the chiral selector and the sample led to good enantiomeric separation. 相似文献