共查询到20条相似文献,搜索用时 46 毫秒
1.
2.
《分析试验室》2017,(7)
采用Penomenex氨基柱为分析柱,建立了高效液相色谱法-蒸发光散射检测方法(HPLC-ELSD)测定油梨种子中不同可溶性糖的方法,并比较了热处理对油梨种子中不同可溶性糖的含量的影响。高效液相色谱分析条件的优化条件为乙腈-水(88:12,体积比)为流动相,流速1.0 mL/min,柱温25℃,氮气压力为172 kPa,漂移管温度为60℃。6种糖标准品线性关系良好。检出限为0.09~0.41 mg/L,样品的加标回收率84.5%~104.7%,相对标准偏差(RSD)小于4.9%。油梨种子中的可溶性糖主要由果糖、葡萄糖、D-甘露庚酮糖和甘露庚糖醇组成;油梨种子经热处理后,其中可溶性糖含量均有所下降。 相似文献
3.
高效液相色谱法测定饮料中糖、甘油和乙醇 总被引:1,自引:0,他引:1
研究了高效液相色谱法测定饮料中糖、甘油和乙醇的方法。饮料样品用WatersSep Pak C18固相萃取小柱预分离 ,以WatersSugar Pak 1钙型阳离子交换柱为固定相 ,0 .0 5 g·L- 1ED TA钙钠水溶液为流动相 ,示差折光仪为检测器 ,一次进样测定饮料样品中的糖、甘油和乙醇。检出限在微克级 ,RSD在 0 .6 8%~ 2 .1%之间 ,标准回收率在 96 %~ 10 7%之间。方法用于几种饮料样品的测定 ,结果满意 相似文献
4.
软骨素酶ABC酶解高效液相法测定鱼翅中的透明质酸 总被引:1,自引:0,他引:1
建立了一种测定鲨鱼翅中透明质酸的酶解 高效液相方法。在37℃,0 2mol/LTris HCl缓冲溶液中,鱼翅中的透明质酸被硫酸软骨素酶ABC酶解成透明质酸二糖。条件为:ZORBAX糖分析柱(4 6mmi d ×250mm,5μm)柱;紫外检测波长226nm;流动相为乙腈 0 5%磷酸(体积比为2∶98),流速1mL/min;进样量10μL。透明质酸二糖的线性范围为25g/L~600g/L。将此法应用到鱼翅的实际样品检测中,取得了良好的结果,透明质酸在鱼翅样品中的质量分数为0 86%~1 96%。 相似文献
5.
建立同时测定浓缩果汁中木糖、果糖、葡萄糖、蔗糖和麦芽糖的高效液相色谱–蒸发光散射检测方法(HPLC–ELSD)。样品采用乙腈–水(50∶50)稀释,用酰胺键合色谱柱BEH Amide分离,蒸发光散射检测器检测,在10 min内完成木糖、果糖、葡萄糖、蔗糖、麦芽糖的分离。浓缩果汁中5种可溶性糖的质量浓度在0.1~2.0 mg/m L与色谱峰面积均呈线性关系,相关系数为0.991 0~0.993 1,检出限为0.23%~0.98%,样品加标回收率为88.6%~104.3%,测定结果的相对标准偏差为2.2%~6.3%(n=6)。该方法快速、准确,可作为浓缩果汁中糖含量的质量控制方法。 相似文献
6.
《分析试验室》2017,(12)
建立了高效液相色谱测定林业生物质原料中可溶性糖的含量和种类的方法。前处理方法为样品称样量4~5g,蒸馏水热浸提1.0 h。色谱条件为:色谱柱(XBridge Amide NUCLEOSIL100-5 NH24.6×250 mm,3.5μm);流动相为V(乙腈):V(水)=83:17,加入0.1%(V/V)的三乙胺;柱温为30℃;流速1.0 m L/min;进样量20μL。在此条件下,葡萄糖、木糖、阿拉伯糖、果糖、甘露糖和蔗糖6种糖的质量浓度分别与峰面积呈良好的线性关系(R20.9978),检测限在3.26~4.30 mg/L之间;加标回收率在96.2%~103.4%之间。对毛竹竹材,油茶饼粕,橡胶树树干,虎榛子树干,胡杨树干,白桦根、枝、树干,马尾松针叶,银杏叶,毛白杨树干等实际样品进行测定时发现,林木生物质的种类、取样部位不同,所含有的可溶性糖种类及含量差异较大。该方法可用于测定林业生物质原料中可溶性糖含量。 相似文献
7.
8.
液相色谱/蒸发光散射测定转基因烟草提取液中的海藻糖 总被引:6,自引:0,他引:6
采用乙二胺动态修饰硅胶柱分离、蒸发光散射检测器测定了转基因烟草提取液中的糖。 4种糖的峰面积标准曲线在 10 0mg/L~ 15 0 0mg/L范围内均具有良好的线性关系。所建立的方法对果糖、葡萄糖、蔗糖、海藻糖的检测下限分别为 10mg/L ,2 0mg/L ,10mg/L和 10mg/L。 相似文献
9.
离子交换固相萃取-高效液相色谱法研究吡虫啉在梨中的分布及残留动态 总被引:3,自引:0,他引:3
建立一种以固相萃取(SPE)、高效液相色谱(HPLC)为基础的测定梨果皮、果肉中吡虫啉残留量的方法。样品用乙腈进行提取,经二氯甲烷液液分配后用阳离子交换固相萃取(SCX-SPE)柱净化,高效液相色谱/二极管阵列检测法(HPLC/DAD)测定。各种添加水平(果皮:0.05、0.1、0.5、2 mg/kg;果肉:0.05、0.5、1mg/kg)的回收率为83%~103%,相对标准偏差(RSD)小于10%,方法的检出限为0.05 mg/kg。运用此方法分别对梨果皮和果肉中吡虫啉的残留动态进行研究,发现吡虫啉主要在梨果皮中残留,得到吡虫啉在果皮中的消解动态方程为:wt=w0×exp(-0.235t),半衰期是2.98 d。 相似文献
10.
11.
An efficient approach to the synthesis of highly congested di, penta and hexacyclic pyrazoles as well as imidazole fragment containing novel heterocyclic molecule has been developed through a carbanion induced transformation of suitably functionalized 2H-pyran-2-ones, benzo[h]chromene and thiochromeno[4,3-b]pyrans. Due to the presence of fluorescence, we report their prime application metal sensor as off/on switching in ferric ions. 相似文献
12.
Uroš Grošelj Mojca Žorž Amalija Golobič Branko Stanovnik Jurij Svete 《Tetrahedron》2013,69(52):11092-11108
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives. 相似文献
13.
The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion. 相似文献
14.
N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%). 相似文献
15.
An efficient tandem approach for the selective synthesis of 4,5-dihydroimidazo[1,5-a]quinoxalines 6a–g and imidazo[1,5-a]quinoxalines 7a–h by the reaction of 2-imidazolyl anilines 4a–c with aryl aldehydes 5a–k under mild reaction conditions is described. Introduction of electron releasing alkyl groups in substrates 4a–b was found to be instrumental for the success of the reaction. 相似文献
16.
The Diels-Alder reactivity of 1,2-heteroborines (H4C4B(H)X, X?=?NH, PH, AsH; O, S, Se) has been computationally explored by means of Density Functional Theory (DFT) calculations. The influence of the HB?=?X fragment on the reactivity of the system has been quantitatively analyzed in detail by means of the so-called Activation Strain Model (ASM) of reactivity. It is found that the interaction between these species and the dienophile is significantly stronger than that computed for their all-carbon isoelectronic counterpart, benzene. In addition, the strain energy plays a key role in the observed reactivity trends. The role of the aromaticity strength of these heteroarenes on the reactivity is also assessed. 相似文献
17.
Xi-Liu YunWen-Ying Bi Jian-Hui HuangYu Liu Daisy Zhang-NegrerieYun-Fei Du Kang Zhao 《Tetrahedron letters》2012,53(38):5076-5080
A variety of N-aryl and N-alkyl carbazolones were conveniently achieved in good to high yields via Pd2(dba)3-mediated intramolecular coupling of N-substituted α-iodo enaminones under microwave irradiation. The Pd(0)-catalyzed cyclization was found to proceed favorably with the more electron-deficient phenyl ring during the reactions involving unsymmetrical N,N-diaryl α-iodo enaminones. This unique property enables the construction of carbazolone skeleton containing nitro substituted benzenoid ring. 相似文献
18.
Shashikant U. Dighe Surya K. Samanta Shivalinga Kolle Sanjay Batra 《Tetrahedron》2017,73(17):2455-2467
An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y1 and Y2. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones. 相似文献
19.
In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates. 相似文献
20.
Both substituted 2,4,5,6-tetrahydrocyclopenta[c]pyrazoles and 2,4,5,6-tetrahydropyrrolo[3,4-c]pyrazoles have been synthesized by the 3+2 intramolecular dipolar cycloaddition of nitrilimines to alkynes. This cyclization has been extended to more versatile 3-bromo derivatives by the use of alkynylbromides as dipolarophiles. 相似文献