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白刺中酚酸类化合物的固相萃取-高效液相色谱快速测定
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作者 陈晨 赵晓辉 +3 位作者 文怀秀 陶燕铎 邵赟 梅丽娟 《时珍国医国药》 CAS CSCD 北大核心 2011年第11期2637-2638,共2页
目的建立固相萃取-高效液相色谱快速测定白刺中3种酚酸(没食子酸、儿茶素、咖啡酸)。方法经过固相萃取后的白刺在色谱条件为:C18柱(4.6 mm×250 mm,5μm),流动相为甲醇-0.2%甲酸缓冲液,流速1 ml/min时进行梯度洗脱。结果 3种酚酸类... 目的建立固相萃取-高效液相色谱快速测定白刺中3种酚酸(没食子酸、儿茶素、咖啡酸)。方法经过固相萃取后的白刺在色谱条件为:C18柱(4.6 mm×250 mm,5μm),流动相为甲醇-0.2%甲酸缓冲液,流速1 ml/min时进行梯度洗脱。结果 3种酚酸类化合物在一定的范围内有良好的线性关系,相关系数均为0.999 9,平均回收率(n=5)分别为96.1%(RSD=1.9%),95.8%(RSD=2.1%),97.4%(RSD=2.2%)。结论通过固相萃取技术以及HPLC法测定3种酚酸类成分的含量,为白刺的质量控制和资源开发提供了切实可行的方法。 展开更多
关键词 高效液相色谱色谱 白刺酚酸 固相萃取
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高效液相色谱法测定生乳中双乙酸钠
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作者 张养东 郑楠 +3 位作者 李松励 郑姗姗 许晓敏 王加启 《中国畜牧兽医》 CAS 北大核心 2013年第S1期37-38,共2页
试验旨在建立高效液相色谱(HPLC)测定生乳中双乙酸钠的方法。生乳样品经磷酸变性沉淀蛋白,并将样品中双乙酸钠酸化转化为乙酸,定容,离心取上清液,过微孔滤膜后,以磷酸二氢铵为流动相进行HPLC检测,外标法定量。在0.05~0.50mg/mL浓度范围... 试验旨在建立高效液相色谱(HPLC)测定生乳中双乙酸钠的方法。生乳样品经磷酸变性沉淀蛋白,并将样品中双乙酸钠酸化转化为乙酸,定容,离心取上清液,过微孔滤膜后,以磷酸二氢铵为流动相进行HPLC检测,外标法定量。在0.05~0.50mg/mL浓度范围内,标准曲线R2=0.997,样品加标回收率在90%~110%之间,相对标准偏差1.0%~4.1%。此方法检出限为0.05g/kg。 展开更多
关键词 高效液相色谱色谱(HPLC) 生乳 双乙酸钠
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κ-卡拉胶寡糖的反相离子对-超高效液相色谱-四极杆-飞行时间质谱研究 被引量:10
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作者 高洋 陈海敏 +2 位作者 徐继林 陈德莹 严小军 《分析化学》 SCIE EI CAS CSCD 北大核心 2009年第11期1590-1595,共6页
建立反相离子对-超高效液相色谱(RPIP-UPLC)和电喷雾离子源-四极杆-飞行时间质谱(ESI-Q-TOF-MS)联用技术快速分离鉴定硫酸寡糖的方法。以20mmol/L庚胺(pH4)为离子对试剂,25%庚胺甲酸盐纯水溶液(A)和25%庚胺甲酸盐甲醇溶液(B)为梯度洗脱... 建立反相离子对-超高效液相色谱(RPIP-UPLC)和电喷雾离子源-四极杆-飞行时间质谱(ESI-Q-TOF-MS)联用技术快速分离鉴定硫酸寡糖的方法。以20mmol/L庚胺(pH4)为离子对试剂,25%庚胺甲酸盐纯水溶液(A)和25%庚胺甲酸盐甲醇溶液(B)为梯度洗脱溶剂,κ-卡拉胶寡糖通过BEHC18反相柱分离后,分别在正、负离子模式下进行四极杆-飞行时间质谱分析。结果表明,聚合度为3~45的κ-卡拉胶寡糖在BEH C18柱上得到很好的分离,从每一个色谱峰对应的质谱图中可以准确获得直至27糖的各寡糖结构信息,均为奇数糖,与聚丙烯凝胶电泳结果吻合。所得的寡糖断裂规律对卡拉胶寡糖的快速鉴定和结构解析具有重要意义。 展开更多
关键词 Κ-卡拉胶 反相离子对-超高效液相 电喷雾离子源-四极杆-飞行时间质 聚丙烯凝胶电泳
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手性固定相色谱柱空隙率的测定研究 被引量:2
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作者 朱磊 刘玉明 +2 位作者 孙玉高 周慧君 徐进 《辽宁化工》 CAS 2012年第1期100-103,共4页
利用高效液相色谱法对硅胶表面涂敷多聚物手性色谱柱空隙率进行测定,并探讨了进样浓度和柱温对测定手性色谱柱死时间的影响。实验以V(正己烷)/V(乙醇)/V(三氟乙酸)=80︰20︰0.01作为流动相,在流速为1.00 mL/min,柱温为25℃,检测波长为25... 利用高效液相色谱法对硅胶表面涂敷多聚物手性色谱柱空隙率进行测定,并探讨了进样浓度和柱温对测定手性色谱柱死时间的影响。实验以V(正己烷)/V(乙醇)/V(三氟乙酸)=80︰20︰0.01作为流动相,在流速为1.00 mL/min,柱温为25℃,检测波长为254 nm,进样量为20μL的条件下,利用不同浓度1,3,5-三叔丁基苯(TTBB)对半制备型手性色谱柱(Chiralpak AD柱)和分析型(ChiralpakAD-H柱)的空隙率进行了测定,结果分别为0.660和0.683。 展开更多
关键词 固定相 手性 高效液相 空隙率测量 死体积
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基于高效液相色谱-高分辨串联质谱的他克莫司软膏杂质谱研究 被引量:1
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作者 布仁 周刚 +4 位作者 盛华 莲花 曹慧敏 朱召贞 白文明 《中国药学杂志》 CAS CSCD 北大核心 2024年第1期78-87,共10页
目的研究他克莫司软膏的杂质谱,为仿制药质量标准制定提供依据。方法采用高效液相色谱-高分辨串联质谱联用技术分析强制破坏后的他克莫司软膏杂质,根据一级、二级质谱数据结合杂质的质谱裂解方式,推测各杂质的来源和分子结构。结果他克... 目的研究他克莫司软膏的杂质谱,为仿制药质量标准制定提供依据。方法采用高效液相色谱-高分辨串联质谱联用技术分析强制破坏后的他克莫司软膏杂质,根据一级、二级质谱数据结合杂质的质谱裂解方式,推测各杂质的来源和分子结构。结果他克莫司软膏强制破坏后,共产生10个杂质,其中包括3组同分异构体。结论本研究建立的杂质谱分析方法为他克莫司软膏的质量控制和工艺优化提供了参考依据。 展开更多
关键词 他克莫司软膏 杂质 裂解方式 高效液相-高分辨串联
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外标法和一测多评法测定忍冬中成分含量的对比研究 被引量:4
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作者 张潇 郭力 +3 位作者 王江瑞 周勤梅 刘宇 陈文仿 《食品研究与开发》 CAS 北大核心 2017年第6期127-132,共6页
对比研究外标对照品法与一测多评法测定传统药食两用忍冬中4种成分含量的差异。采用外标对照品法测定不同产地忍冬中4种成分的含量,分别以绿原酸和芦丁为参照物建立与其余成分的相对校正因子,实现一测多评,比较外标法与"一测多评&q... 对比研究外标对照品法与一测多评法测定传统药食两用忍冬中4种成分含量的差异。采用外标对照品法测定不同产地忍冬中4种成分的含量,分别以绿原酸和芦丁为参照物建立与其余成分的相对校正因子,实现一测多评,比较外标法与"一测多评"的结果,以验证"一测多评"法的准确度及可行性。结果表明:一测多评应法用于不同产地忍冬中不同类型化合物的含量测定存在显著性差异,应用于不同产地忍冬中同类型化合物的含量测定不存在显著性差异。一测多评法不适用于忍冬中不同类型化合物之间含量测定,其应用有一定局限性。 展开更多
关键词 一测多评 忍冬 相对校正因子 高效液相色谱色谱
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迪娜尔合剂的化学成分预检识及含量测定
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作者 乃比江·麦图荪 买买提明·买合木提 艾尼娃尔·艾克木 《新疆医科大学学报》 CAS 2024年第9期1288-1292,1300,共6页
目的预检识迪娜尔合剂的化学成分,测定绿原酸和咖啡酸的含量。方法采用化学反应鉴别法对迪娜尔合剂中的化学成分类型进行鉴别检识;采用福林酚法测定迪娜尔合剂中总多酚的含量;采用薄层色谱法(TLC)对迪娜尔合剂进行定性鉴别分析;采用高... 目的预检识迪娜尔合剂的化学成分,测定绿原酸和咖啡酸的含量。方法采用化学反应鉴别法对迪娜尔合剂中的化学成分类型进行鉴别检识;采用福林酚法测定迪娜尔合剂中总多酚的含量;采用薄层色谱法(TLC)对迪娜尔合剂进行定性鉴别分析;采用高效液相色谱法(HPLC)对迪娜尔合剂中的绿原酸与咖啡酸含量进行测定。结果迪娜尔合剂富含多种生物活性化合物,包括糖类、香豆素类、生物碱类、酚类化合物和有机酸类化合物。迪娜尔合剂中总多酚含量为(1.57±1.71)mg/mL,绿原酸和咖啡酸两种单体成分的含量分别为(94.17±0.23)μg/mL和(0.27±0.45)μg/mL。结论迪娜尔合剂中含有多种生物活性化合物,其中多分酚类化合物含量较高,本研究为迪娜尔合剂的质量控制和疗效评估提供了科学依据。 展开更多
关键词 迪娜尔合剂 预检识 总多酚 薄层:高效液相
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尿中修饰核苷代谢轮廓分析在肺癌诊断中的作用 被引量:6
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作者 王文昭 赵欣捷 +3 位作者 李响 陈静 李方楼 许国旺 《中国医学科学院学报》 CAS CSCD 北大核心 2007年第6期738-741,共4页
目的探讨尿中修饰核苷代谢轮廓分析在肺癌诊断中的作用。方法应用二维液相色谱在线分析系统得到42名正常人和80例肺癌患者尿中修饰核苷代谢轮廓谱,结合偏最小二乘判别分析法(PLS-DA)对所得到的代谢轮廓谱数据进行分析。结果尿中修饰核... 目的探讨尿中修饰核苷代谢轮廓分析在肺癌诊断中的作用。方法应用二维液相色谱在线分析系统得到42名正常人和80例肺癌患者尿中修饰核苷代谢轮廓谱,结合偏最小二乘判别分析法(PLS-DA)对所得到的代谢轮廓谱数据进行分析。结果尿中修饰核苷代谢轮廓谱分析结合PLS-DA数据处理方法可以用于区分正常人与肺癌患者,其模型判断预测值为Q2=0.744。讨论尿中修饰核苷代谢轮廓分析对肺癌的诊断有一定的参考意义。 展开更多
关键词 尿中修饰核苷 高效液相亲和在线系统法 偏最小二乘判别分析 代谢轮廓分析
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Polyphenols from Vitis thunbergii Sieb. et Zucc. 被引量:1
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作者 窦德强 任杰 +7 位作者 Maggie Cooper 何曜华 裴玉萍 Yoshiaki Takaya Masatake Niwa 陈英杰 姚新生 周仁平 《Journal of Chinese Pharmaceutical Sciences》 CAS 2003年第2期57-59,共3页
Aim Isolation and structural elucidation of the constituents from the aerial part of Vitis thunbergii . Methods To isolate chemical constituents, column chromatography and HPLC were used. Physico chemical ... Aim Isolation and structural elucidation of the constituents from the aerial part of Vitis thunbergii . Methods To isolate chemical constituents, column chromatography and HPLC were used. Physico chemical characterization and spectroscopic analysis were employed for structural identification. Results Eleven polyphenols were isolated and identified. Conclusion Compound 1 is a new compound and its structure was characterized to be 3,5 dimethoxyl 4 hydroxyl phenylpropanol 9 O β D glycopyranoside. 展开更多
关键词 Vitis thunbergii phenylpropanol glycoside POLYPHENOL
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Optimization of Chromatographic Conditions for Detecting Ellagic Acid in Pomegranate Peels Using HPLC Method 被引量:3
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作者 夏小龙 彭蓉 +3 位作者 李树垠 李端阳 干霞 白琦 《Agricultural Science & Technology》 CAS 2012年第11期2400-2403,共4页
[Objective] This study aimed to optimize the chromatographic conditions for detecting ellagic acid in pomegranate peels using HPLC method. [Method] By using 0.2 mg/ml ellagic acid standard solution, on the basis of si... [Objective] This study aimed to optimize the chromatographic conditions for detecting ellagic acid in pomegranate peels using HPLC method. [Method] By using 0.2 mg/ml ellagic acid standard solution, on the basis of single-factor experiment and orthogonal experiment, chromatographic conditions (mobile phase ratio, flow rate, col- umn temperature) for detecting ellagic acid using HPLC were optimized. Based on the optimal chromatographic conditions, the ellagic acid content in experimental pomegranate peels was determined. [Resull] The optimal chromatographic conditions for detecting ellagic acid in pomegranate peels using HPLC method are: 1.2% phos- phoric acid:acetonitrile=85:15, column temperature of 35 ℃, and flow rate of 1.0 ml/min. The linear regression equation of ellagic acid is: y=2.9e+0.6x+4.4e+5 (FF=9 999). Ac- cording to the standard addition recovery test, the average recovery rate of ellagic acid is 98.20%, and RSD is 0.60%. Under above optimized chromatographic condi- tions, ellagic acid can be well separated from other interfering components in pomegranate peels, with shorter peak time and ideal effect, which is convenient for the detection in production practices. [Conclusion] This study laid the foundation for detecting ellagic acid in pomegranate peels using HPLC method. 展开更多
关键词 Pomegranate peel Etlagic acid DETECTION HPLC
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Identification of Qishen Oral Solution with TLC and HPLC 被引量:1
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作者 王建舫 茹颖楠 +2 位作者 宋晶 朱迪凡 穆祥 《Agricultural Science & Technology》 CAS 2013年第12期1834-1838,共5页
[Objective] This study aimed to establish the standards for quality control of Qishen oral solution. [Method] Astragalus membranaceus, Atractylodes macro- cephala Koidz. and Glycyrrhiza uralensis in the preparation we... [Objective] This study aimed to establish the standards for quality control of Qishen oral solution. [Method] Astragalus membranaceus, Atractylodes macro- cephala Koidz. and Glycyrrhiza uralensis in the preparation were identified by using thin layer chromatography (TLC), and Codonopsis pilosula was identified by using high-performance liquid chromatography (HPLC). [Result] By using the developed TLC system, experimental solution and reference solution showed clear spots, while negative control presented no interference. By using the developed HPLC system, the chromatographic peak of Iobetyolin was detected in experimental solution. [Con- clusion] The developed TLC and HPLC systems presented high specificity and good repeatability for identification of these four components and could be used in the quality control of Qishen oral solution. 展开更多
关键词 Qishen oral solution TLC LOBETYOLIN HPLC
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大豆异黄酮酶解物中活性成分的薄层鉴别及含量测定 被引量:1
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作者 李剑梅 修翠娟 +1 位作者 李莉 张玉东 《现代畜牧兽医》 2007年第2期4-7,共4页
采用GF254薄层色谱鉴别方法对大豆异黄酮酶解产物中的大豆苷元和染料木素进行快速鉴别,同时用HPLC法对其活性成分进行了含量测定。结果表明:在同一薄层板上与标准大豆苷元、染料木素荧光斑点对应的位置上,大豆异黄酮酶解物有色泽相同的... 采用GF254薄层色谱鉴别方法对大豆异黄酮酶解产物中的大豆苷元和染料木素进行快速鉴别,同时用HPLC法对其活性成分进行了含量测定。结果表明:在同一薄层板上与标准大豆苷元、染料木素荧光斑点对应的位置上,大豆异黄酮酶解物有色泽相同的荧光斑点,Rf分别为0.3、0.6,该方法斑点明显、重现性好、专属性强,能对转化结果进行准确的定性判断。采用HPLC法测定活性成分的含量,在一定的浓度范围内,标准样品的浓度和吸收峰面积呈良好的线性关系(r值均大于0.99),HPLC图谱清晰、峰形稳定,保留时间较为理想,各个组分间的分离度均大于1.5,且精密度高,加标回收率在99%以上,能同时测定大豆异黄酮4组分的含量。大豆异黄酮酶解物中大豆苷、大豆苷元、染料木苷、染料木素的含量分别为:0.129%、4.101%、0.028%、1.442%。 展开更多
关键词 薄层(TLC)高效液相(HPLC) 大豆异黄酮酶解物 大豆苷
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Determination of astaxanthin and astaxanthin esters in shrimp shell by HPLC 被引量:8
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作者 LI Shuai GUO Jun-ru +6 位作者 FENG Jin-hua ZHU Ze-min LI Ling-li GUO Xiao-fang SUI Wen-yan WANG Meng ZUO Wen-ting 《Marine Science Bulletin》 CAS 2019年第2期57-71,共15页
A method for determination of astaxanthin and astaxanthin eaters in shrimp shell by high performance liquid chromatography is established.Shrimp shell are addressed with 5%hydrochloric acid to remove calcium ions.Afte... A method for determination of astaxanthin and astaxanthin eaters in shrimp shell by high performance liquid chromatography is established.Shrimp shell are addressed with 5%hydrochloric acid to remove calcium ions.After shell is dried,organics from shrimp shell are extracted with anhydrous ethanol.The alcohol extrative of the shrimp shell is mixed with the ammonium sulfate to extract astaxanthin by aqueous two-phase extraction.The crude astaxanthin is collected,which is distributed in the middle layer of the aqueous two-phase layer.After distilled water is added to the crude astaxanthin,the aqueous solution is centrifuged,and the previous step is repeated for several times.The precipitation in centrifuge tube is collected and dried.The crude astaxanthin dried is dissolved with acetone,and the sample solution is separated by TLC.Every pigment on the TLC plate is collected and dissolved with acetone.The pigments are determined by high performance liquid chromatograph.The results show that aqueous two-phase system,3 mL alcohol extractive of astaxanthin and 4.5 mL 20%ammonium sulfate,can be used to acquire crude astaxanthin.The wavelength of the maximum peak of astaxanthin in ethanol solution is 472 nm.A variety of pigments can be separated from the crude astaxanthin by thin-layer chromatography,including free astaxanthin,astaxanthin monoester,astaxanthin diester,echinenone and other substances.It can be seen from high performance liquid chromatography that the appearance time of free astaxanthin is from 4 min to 5.5 min,and the appearance time of astaxanthin monoester is from 10.5 min to 27.8 min.The method is simple about the sample pretreatment and feasible about the determination of astaxanthin and astaxanthin esters in shrimp shell. 展开更多
关键词 ASTAXANTHIN astaxanthin esters aqueous two-phase thin-layer chromatography high performance liquid chromatography
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酱香型白酒轮次基酒中非挥发性风味物质的差异研究 被引量:4
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作者 骆茂香 陈仁远 +1 位作者 徐兴江 邱树毅 《食品与发酵工业》 CAS CSCD 北大核心 2023年第19期282-288,I0005,共8页
利用超高效液相色谱(ultra performance liquid chromatography,UPLC)和超高效液相色谱串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)两种分析方法对大曲酱香一至七轮次及综合基酒中非挥发... 利用超高效液相色谱(ultra performance liquid chromatography,UPLC)和超高效液相色谱串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)两种分析方法对大曲酱香一至七轮次及综合基酒中非挥发性有机酸类及酚酸物质进行定性定量分析,结合化学计量方法构建辨识模型,并找出关键差异化合物。结果表明:在酱香型酒轮次基酒及综合基酒中均检出18种非挥发性风味物质,但18种化合物含量各有不同。其中,乳酸在一至七轮次及综合基酒中含量均远高于其他17种非挥发性组分。检出的18种物质在一至七轮次及综合基酒中的含量变化趋势亦有所不同。采用主成分分析级正交偏最小二乘判别分析法构建了酱香型白酒一至七轮次基酒及综合基酒的鉴别模型。变量投影重要性(variable importance in projection,VIP)分析筛选出5种可用于区分不同轮次及综合基酒的潜在差异物质,即乳酸、油酸、亚油酸、马来酸及阿魏酸,乳酸VIP值(2.6286)最高,说明乳酸对于区分不同轮次基酒酒样贡献最大,该模型可基本实现酱香型白酒不同轮次基酒及综合基酒中非挥发性有机酸及酚酸的差异评价。通过单因素方差分析发现:5种关键化合物在不同轮次基酒中有不同的变化趋势,它们在含量最高和最低的轮次基酒中存在显著差异(P<0.05),但在相邻轮次间会存在显著差异(P<0.05)或不显著差异(P>0.05)的变化趋势。进一步验证通过化学计量学方法筛选出的5种潜在差异物质的含量在不同轮次存在共性与个性。 展开更多
关键词 不同轮次大曲酱香型白酒 高效液相及超高效液相串联质 非挥发性物质 化学计量学 差异分析
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岩果止咳液质量标准改进 被引量:1
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作者 吕情花 《中国药业》 CAS 2020年第7期116-118,共3页
目的改进岩果止咳液的质量标准。方法采用薄层色谱(TLC)法对果上叶进行定性鉴别;采用高效液相色谱-紫外检测(HPLC-UV)法同时测定石吊兰、甘草流浸膏中石吊兰素、甘草酸铵的含量。结果TLC斑点清晰,专属性强;石吊兰素、甘草酸铵质量浓度... 目的改进岩果止咳液的质量标准。方法采用薄层色谱(TLC)法对果上叶进行定性鉴别;采用高效液相色谱-紫外检测(HPLC-UV)法同时测定石吊兰、甘草流浸膏中石吊兰素、甘草酸铵的含量。结果TLC斑点清晰,专属性强;石吊兰素、甘草酸铵质量浓度分别在0.004866~0.2433 mg/mL(r=0.9999)和0.0228~1.140 mg/mL(r=0.9997)范围内与峰面积线性关系良好,平均加样回收率分别为98.46%和98.91%,RSD分别为2.25%和0.98%(n=9)。结论该方法灵敏、准确,可完善岩果止咳液的质量标准。 展开更多
关键词 岩果止咳液 果上叶 石吊兰素 甘草酸铵 高效液相-紫外
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Fucoxanthin Content of Five Species Brown Seaweed from Talango District, Madura Island 被引量:1
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作者 K. Zailanie H. Purnomo 《Journal of Agricultural Science and Technology(A)》 2011年第8期1103-1105,共3页
Fucoxanthin content of five brown seaweed species of East Java collected from Talango district (Madura sea-Jawa sea) namely Padina australis, Turbinaria conoides, Sargassum cinereum, Sargassum filipendula and Sargas... Fucoxanthin content of five brown seaweed species of East Java collected from Talango district (Madura sea-Jawa sea) namely Padina australis, Turbinaria conoides, Sargassum cinereum, Sargassum filipendula and Sargassum echinocarpum were determined and samples were collected using Global Positioning System (GPS). Fucoxanthin from those samples was determined using Thin Layer Chromatography (TLC), High Pressure Liquid Chromatography (HPLC) and Spectrophotometer UV-Vis and the results were then calculated using Seely equation. The pigments separation using HPLC gave a better result compared to TLC, and beside fucoxanthin otlher pigments namely chlorophyll and β carotene were also identified in these samples. Four points of sampling location were chosen using GPS and spot with coordinate positions observed were 113.94444° EL-7.08795° SA; 113.94231° EL-7.08913° SA. The results showed that fucoxanthin content were as follow: Padina australis 0.2674± 0.0046 mg/g; Turbinaria conoides 0.2134± 0.0100 mg/g; Sargassum filipendula 0.1957 ± 0.0173 mg/g; Sargassum cinereum 0.1640 ± 0.0092 mg/g and Sargassum echinocarpum 0.1576 ± 0.0001 mg/g. It can be concluded that Padina australis and Turbinaria conoides contain the most amount of fucoxanthin and it is possible to be cultivated as edible brown seaweed fucoxanthin resources. 展开更多
关键词 Fucoxan thin brown seaweed Madura Island
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3-脱氧葡萄糖醛酮代谢产物——3-脱氧果糖的HPLC检测方法初步建立
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作者 李涵艺 江国荣 +2 位作者 许恒 季亚男 张露蓉 《纤维素科学与技术》 CAS 2023年第1期16-22,共7页
建立了3-脱氧果糖(3-DF)初步检测的高效液相色谱(HPLC)方法。先使用气相色谱―质谱联用(GC-MS)对合成的3-DF标样进行鉴定。再采用C18反相色谱柱,流动相为乙腈-水(10%∶90%~90%∶10%)梯度洗脱60min,紫外检测波长352nm,应用2,4-二硝基苯... 建立了3-脱氧果糖(3-DF)初步检测的高效液相色谱(HPLC)方法。先使用气相色谱―质谱联用(GC-MS)对合成的3-DF标样进行鉴定。再采用C18反相色谱柱,流动相为乙腈-水(10%∶90%~90%∶10%)梯度洗脱60min,紫外检测波长352nm,应用2,4-二硝基苯肼柱前衍生法,以薄层色谱―高效液相色谱联用(TLC-HPLC)对3-DF衍生物峰进行定位,并完善衍生条件,进行方法学考察。结果表明:合成样品为3-DF;衍生条件以衍生液中1∶3添加乙酸乙酯效果最佳;3-DF衍生物峰出峰时间为15.972 min,呈尖峰,分离度良好,线性范围为0.5~8 mg/mL,方法精密度RSD为2.4%,重复性RSD为4.4%,稳定性RSD为2.4%。本检测方法稳定、可靠,可初步用于3-DF定性及相对定量。 展开更多
关键词 3-脱氧果糖 3-脱氧葡萄糖醛酮 2 4-二硝基苯肼 高效液相 气相―质联用 薄层高效液相联用
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Economic and Qualitative Traits of Italian Alps Saffron 被引量:1
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作者 Alessandra MANZO Sara PANSERI +1 位作者 Danilo BERTONI Annamaria GIORGI 《Journal of Mountain Science》 SCIE CSCD 2015年第6期1542-1550,共9页
Saffron, obtained from the flower stigmas of Crocus sativus L., is one of the most expensive food spices. The introduction of saffron in alpine areas could help to broaden and diversify the activities of mountain mult... Saffron, obtained from the flower stigmas of Crocus sativus L., is one of the most expensive food spices. The introduction of saffron in alpine areas could help to broaden and diversify the activities of mountain multifunctional farms, with a positive impact on economy and land management. According to ISO 3632(2010/2011), saffron can be classified into three categories of quality(I, II, III) depending on the concentration of the three main metabolites responsible for its characteristic colour, flavor and aroma: Crocin, Picrocrocin and Safranal. This study represents the first investigation of the quality of saffron produced in the Italian Alps evaluated with spectrophotometry, HPLC, solid-phase microextraction(SPME), and gas chromatographic analysis combined with mass spectrometry(GC/MS). The experiments used Crocus sativus stigmas produced in 2012-2013 in different areas of the Central Italian Alps were located at an altitude between 720 and 1200 m a.s.l.. Results obtained were compared to commercial saffron. The analyses confirmed that all samples can be classified in the first quality category according to the ISO classification. This high quality is also confirmed by HPLC analysis. Moreover, the SPME-GC/MS analysis identified some differences in the aromatic profile of saffron samples, in particular regarding safranal concentration. A preliminary assessment of the economic viability of high quality saffron production for local markets was also performed. Our study provides valid information regarding the quality and economic sustainability of saffron production in the alpine area confirming this crop as a good candidate for a new source of income for multifunctional farms in mountain areas. 展开更多
关键词 Crocus sativus L. Alps ISO 3632 UV– Vis spectrophotometry SPME-GC/MS HPLC
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Qualitative and Quantitative Analysis of Linoleic Acid in Polygonati Rhizoma 被引量:1
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作者 ZHOU Zhun YUAN Han-Wen +8 位作者 PENG Cai-Yun JIAN Yu-Qing ZHOU Xu-Dong LI Bin SHENG Wen-Bing GONG Li-Min HE Shu-Jin WANG Wei LIU Chang-Xiao 《Digital Chinese Medicine》 2020年第3期180-187,共8页
Objective To explore the major compound in Polygonati Rhizoma(Huang Jing,黄精)for quality control.Methods The major compound was isolated and analyzed by liquid chromatography-mass spectrometry(LC-MS),and subsequently... Objective To explore the major compound in Polygonati Rhizoma(Huang Jing,黄精)for quality control.Methods The major compound was isolated and analyzed by liquid chromatography-mass spectrometry(LC-MS),and subsequently further identified by nuclear magnetic resonance(NMR).Thin layer chromatography(TLC)was optimized based on the previous methods reported in the Chinese Pharmacopeia(2015 edition).Results The major compound was isolated from the natural material and identified as linoleic acid.A high performance liquid chromatography(HPLC)method with robust linearity(R2=0.9997),specificity,precision,stability,repeatability and recovery was developed for linoleic acid determination.TLC chromatogram was improved significantly after optimization for qualitative analysis.Conclusions The optimized TLC method is practical and can be adopted for quality control of Polygonati Rhizoma(Huang Jing,黄精).The levels of linoleic acid vary between species of Polygonati Rhizoma(Huang Jing,黄精),with Polygonatum cyrtonema Hua(Jiang Xing Huang Jing,姜型黄精)showing the highest contents.This study provides valuable information for quality control of Polygonati Rhizoma(Huang Jing,黄精). 展开更多
关键词 Polygonati Rhizoma(Huang Jing 黄精) Linoleic acid Qualitative analysis Quantitative analysis Thin layer chromatography(TLC) High performance liquid chromatography(HPLC)
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Changes of Metabolites and Macro- and Micro-elements in Hungarian Potatoes under Organic and Conventional Farming
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作者 Rita Tomoskozi-Farkas Nora Adanyi +6 位作者 Magdolna Gasztonyi-Nagy Maria Berki Viola Horvath Tibor Renkecz Kinga Simon Zoltan Fabulya Zsolt Polgar 《Journal of Agricultural Science and Technology(B)》 2016年第2期83-92,共10页
To study the effect of cultivation system (conventional and organic) on potato tuber components, 42 parameters (anti-nutritives, micro- and macro-elements and 23 metabolites) were studied in three multi-resistant ... To study the effect of cultivation system (conventional and organic) on potato tuber components, 42 parameters (anti-nutritives, micro- and macro-elements and 23 metabolites) were studied in three multi-resistant Hungarian potato varieties for three years in 2007-2009. Discriminant analysis of data proved that all investigated factors (farming technology, genotype and season/year) had significant effect on metabolites. Reversed phase high performance liquid chromatographic (HPLC-DAD, HPLC-MS) and elemental analysis methods have been adapted to quantify the major components, i.e., steroidal alkaloids, nitrite, nitrate, sugars, amino acids and micro-elements, in potato tubers. The absolute amount and changes of tuber components were influenced differentially by the technology, genotype and season in a complex manner. Any examined component, except nitrate content, was found to be significantly higher or lower consistently in relation to the production practice (organic or conventional) during the three years trials. Under the examined circumstances, no consequent positive effect of organic fanning on the total amount of anti-nutritive components, vitamins or micro- and macro-elements of potato tubers could be proven. 展开更多
关键词 POTATO organic farming conventional fanning metabolomics macro- and micro-elements.
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