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反相高效液相色谱-蒸发光散射检测法测定安宫牛黄胶囊中的胆酸 总被引:8,自引:0,他引:8
应用反相高效液相色谱-蒸发光散射检测法对安宫牛黄胶囊中的胆酸含量进行了测定。色谱柱用JASCO C18柱(250 mm×4.6 mm i.d.,5 μm),流动相为甲醇-0.1%(体积分数)醋酸水溶液(体积比为9∶1),流速1.0 mL/min,柱温为室温;蒸发光散射检测器漂移管温度40 ℃,载气(N2)流速4.0 L/min。在上述条件下测得胆酸的进样量为0.50-5.02 μg时线性关系良好(r=0.999?3),最低检测限达到0.05 μg,平均加样回收率为97.1%。该方法快速简捷,精密度高,重现 相似文献
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联合运用高效液相色谱法和管碟法分析牛黄解毒片中抑菌物质黄芩苷、甘草苷。以Diamonsil C18柱(250mm×4.6 mm,5μm)为分析柱,0.15%磷酸水溶液为流动相A、乙腈为流动相B,流量为1.0 mL/min,检测波长为280nm,柱温为30℃,进样体积为10μL。采用高效液相色谱法测定12批不同厂家的牛黄解毒片,记录色谱图;运用《中药色谱指纹图谱相似度评价系统》(2012年版)建立指纹图谱,并进行相似度评价和共有峰指认。采用管碟法,以阿莫西林为对照,测定牛黄解毒片对金黄色葡萄球菌的抑菌活性;使用SPSS 21.0软件对牛黄解毒片的抑菌活性指标值与指认峰峰面积进行灰色关联度分析。建立高效液相色谱指纹图谱,12批不同厂家牛黄解毒片的相似度均不低于0.937,并确认甘草苷与黄芩苷为共有峰;甘草苷的灰色关联度值为0.696,黄芩苷的灰色关联度值为0.680。黄芩苷与甘草苷是牛黄解毒片中的2种抑菌物质。 相似文献
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鉴于韩国已对鱼肉中胆汁酸的残留量进行了相关规定,提出了题示方法。取鱼肉样品5.0 g,加入100μg·L^(-1)胆酸-d_(4)(胆酸内标物)、脱氧胆酸-d_(4)(脱氧胆酸及脱氢胆酸的内标物)混合内标溶液0.1 mL,乙腈20 mL,混匀后超声提取10 min,离心5 min,重复提取一次。合并上清液,旋干,残渣用50%(体积分数,下同)甲醇溶液1 mL超声溶解5 min,加入正己烷5 mL,离心5 min,弃掉正己烷层。保留相过活化好的HLB固相萃取柱,用3 mL水淋洗,抽干柱子,用3 mL甲醇洗脱。收集前5 mL洗脱液,于40℃氮吹至干,残渣用50%甲醇溶液1 mL复溶,过0.45μm滤膜,滤液按照优化的仪器工作条件测定。以Waters ACQUITY UPLC BEH C_(18)色谱柱为固定相,以不同体积比的水和甲醇的混合液为流动相进行梯度洗脱,分离后的目标物用串联质谱仪在电喷雾离子源负离子(ESI^(-))模式下电离,多反应监测(MRM)模式下检测,内标法定量。结果显示:胆酸、脱氧胆酸和脱氢胆酸标准曲线的线性范围均为10~500μg·L^(-1),检出限为0.003 mg·kg^(-1)。对阴性鱼肉样品进行3个浓度水平的加标回收试验,回收率为82.2%~115%,测定值的相对标准偏差(n=6)为2.6%~14%。 相似文献
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胆酸和脱氧胆酸分子的远红外与THz吸收光谱研究 总被引:1,自引:0,他引:1
胆酸和脱氧胆酸是胆汁酸中的主要成分, 是人体中重要的生物表面活性剂. 两种分子只相差一个羟基, 在远红外和太赫兹波段有不同的吸收光谱. 胆酸分子的太赫兹(THz)吸收光谱有1.26 THz(42 cm-1)和2.02 THz(67 cm-1)两个吸收峰, 脱氧胆酸分子的THz吸收光谱有1.13, 1.26, 1.69和2.17 THz(即38, 42, 56, 72 cm-1)等几个吸收峰. 两个分子的THz吸收光谱都包含有1.26 THz(42 cm-1) 峰, 反映出二者结构的相似性. 它们的远红外光谱都有部分频率相近的谱带, 但对比之下可以观察到峰位位移和相对峰强的改变. 指认了两种物质的某些可能与羧基振动有关的特征吸收峰. 为找出THz光谱隐含的信息, 利用Omnic程序采用二阶导数方法来处理THz光谱数据, 观察到多个子峰, 说明分子结构中可能存在更复杂的氢键状态. 实验结果表明, 远红外和THz吸收光谱是研究生物分子及鉴别生物分子结构的很好方法. 相似文献
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胆酸酯及其甲基丙烯酸衍生物的制备 总被引:1,自引:0,他引:1
以HCl为催化剂,合成了脂肪族二元醇单胆酸酯(2~5)。运用甲基丙烯酰氯和甲基丙烯酸酐作酰化试剂,三乙胺作缚酸剂,4-(二甲氨基)吡啶作催化剂,合成了分子中含有不同数量甲基丙酰基的胆酸衍生物(6~9)。实验结果表明,当用甲基丙烯酰氯作酰化剂时,2~5分子中羟基的反应活性顺序是:CH2-OH>3-OH>12-OH>7-OH。 相似文献
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建立了毛细管电泳高频电导法快速简便测定牛黄粉中胆酸的新方法.考察了电泳介质的种类、浓度、 pH值以及操作电压和进样时间对分离检测的影响.缓冲液为0.5 mmol/L Na3PO4 2 mmol/L Na2HPO4 0.2 mmol/L CTAB(pH 11.7), 分离电压为 -15 kV时可实现较好的分离和检测.胆酸的线性范围为75~200 μg/mL, 检出限为0.1 μg/mL.线性方程为y=0.6054ρ-4.14991, r=0.953.回收率为100.9%, RSD(n=5)=2.1%. 相似文献
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采用非等温DSC法分别对3,7,12–三甲基丙烯酰基胆酸甲酯(CAME3MA)和2-甲基丙烯酰氧基-3,7,12-三甲基丙烯酰基胆酸乙酯(CAGE4MA)的固化反应进行了研究,并与2-甲基丙烯酰氧基-3-甲基丙烯酰基胆酸乙酯(CAGE2MA)固化体系进行了比较。结果显示,3个体系有相似的非等温固化曲线,但是相同升温速率的峰顶温度不同,C=C数量越多,放热峰温度越高。用Kissinger法处理非等温DSC数据,3个体系的Ea和lnA值有差别,变化趋势均为CAGE2MA>CAGE4MA>CAME3MA。由于CAGE2MA容易形成分子间氢键,因此它反应所需的活化能也比后两者大;CAME3MA的分子间作用力稍小于CAGE4MA,因此前者的固化反应活化能也比后者略低。 相似文献
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Ethylenediaminetetra-acetic acid (EDTA) and nitrilotri-acetic acid (NTA) can be differentiated and determined by titration with metal ions to visual metallochromic dye end-points. EDTA can be determined without interference from NTA, either by titrating with copper(II) at pH 5 using PAN indicator, or by titrating with iron(III) at pH 6 and 70 degrees using Tiron indicator. The total chelating power (EDTA + NTA) can be determined either by titrating with lead(II) at pH 4.4 using dithizone indicator, or by titrating with iron(III) at pH 3.5 using Tiron indicator ; NTA is determined by difference. The lowest concentration at which NTA can be determined in EDTA by titration to the iron(III)-Tiron end-point is about 1 wt.%. The apparent stability constants of the iron(III)-Tiron complexes under the conditions of the titration at pH 3.5 and pH 6 have been determined using the method of continuous variations. 相似文献
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4-Oxoazetidin-2-ylphosphonates and phosphinates, obtained from Arbusov reactions of 4-acetoxyazetidin-2-one and 4α-acetoxy-3β-phthalimido-2-one with a variety of phosphites and phosphonites, were hyrdolysed to β-phosphono- and β-phosphino β-alanine (phosphono- and phosphinoaspartic acid) derivatives. In model studies for their incorporation in peptides, conditions for the selective removal of protecting groups for carboxylic acids, phosphonic and phosphinic acids, and amines, in derived di- and tri-peptides were investigated. Alanyl and alanyl alanyl peptide incorporation into bacteria was studied. 相似文献
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The equilibrium structures and harmonic vibrational frequencies of peroxynitric acid (HOONO(2)) and seven structures of protonated peroxynitric acid, along with peroxynitrous acid (HOONO) and its 12 protonated peroxynitrous acid structures, have been investigated using several ab initio and density functional methods. The ab initio methods include second-order Moller-Plesset perturbation theory, quadratic configuration interaction, including single and double excitations theory (QCISD), and the QCISD(T) methods, which incorporate a perturbational estimate of the effects of connected triple excitation. The Becke three-parameter hybrid functional combined with Lee, Yang, and Parr correlation function is the density functional method used. The lowest energy form of protonated peroxynitric acid is a complex between H(2)O(2) and NO(+) rather than between H(2)O and NO(2) (+). For peroxynitrous acid, a complex between H(2)O(2) and NO(2) (+) is found to be the lowest energy structure. The ab initio proton affinity (PA) of HOONO and HOONO(2) is predicted to be 182.1 and 175.1 kcal mol(-1), respectively, at the QCISD(T)/6-311++G(3df,3pd) level of theory. The results are contrasted with an earlier study on nitrous acid, and is shown that peroxynitric acid and peroxynitrous acid have a smaller PA than nitrous acid. 相似文献
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Xu Lingling Yang Hongying Liu Yajie Zhou Yipeng 《Journal of Radioanalytical and Nuclear Chemistry》2019,321(3):815-822
Journal of Radioanalytical and Nuclear Chemistry - Citric acid and oxalic acid, the main metabolites of fungi, have different leaching effects on uranium ore. Herein, uranium leaching from a... 相似文献