原创《茄尼醇同步提取皂化—超高效液相色谱测定方法》：本论文主要论述了高效液相色谱论文范文相关的参考文献,对您的论文写作有参考作用。
摘 要：为了建立高效、准确检测烟草总茄尼醇的方法,研究了超声辅助条件下,同步提取、皂化烟草茄尼醇的溶剂、温度、液料比、皂化剂用量、提取时间及超高效液相色谱测定的仪器条件.结果表明,烟草样品以正己烷为萃取剂,液料比为50：1,0.1 moL/L氢氧化钠的乙醇溶液为皂化剂,在超声频率45 kHz,恒温水浴40 ℃,提取时间30 min条件下,完成烟草茄尼醇的提取、皂化,且使茄尼醇的提取、皂化以及和皂化剂的分离在同一离心管中完成.以ACQUITY UPLC BEH C18为色谱柱,甲醇-乙腈（50：50）为流动相,流速为0.5 mL/min,柱温为35 ℃,在波长208 nm条件下,超高效液相色谱进行检测.方法的线性范围为0.67～84.1 mg/L,方法检出限为0.07 mg/L,定量限为0.012%,空白及样品加标回收率分别在97.9%～104.7%、93.4%～102.3%范围内,相对标准偏差为1.34%～2.43%.该方法简便、快速,且节约有机溶剂,精密度和准确度较高,可以实现烟草茄尼醇批量高效检测.
关键词：茄尼醇；提取；皂化；超高效液相色谱
中图分类号：TS411 文章编号：1007-5119（2015）05-0079-06 DOI：10.13496/j.issn.1007-5119.2015.05.015
Abstract： In order to established the method of determining total solanesol in tobacco efficiently and accurately ,we studied the conditions of simultaneously extracting and saponifying solanesol from tobacco, including solvent, temperature, liquid ratio, saponification dosage, extraction time and ultrasound-assisted instruments conditions of ultra-high performance liquid chromatography. Hexane was used as solvent for extraction with liquid-material ratio of 50：1 and 0.1 moL/L sodium hydroxide in ethanol solution was used as saponification agent. The ultrasonic frequency used was 45 kHz, temperature of extraction and saponification was 40 ℃, and time of extraction was 30 min. Under this condition, extracting and saponifying solanesol from tobacco were finished simultaneously, and saponification agent separation was done in the same centrifuge tube. The separation of target compound was performed on an ACQUITY UPLC BEH C18 column using methanol-acetonitrile （50：50） as mobile phase by gradient elution. Flow rate was set at 0.5 mL /min, column temperature was 35 ℃ and injection volume was 5 μL. The quantitative wavelength of UV detector was set at 208 nm. The results indicated that the calibration curve was linear in the range o f 0.67-84.1 mg/L, the limit of detection （LOD, S/N等于3） was 0.07 mg /L, and the limit of quantification （LOQ, S/N等于10） was 0.012%. The standard addition recoveries of blanks and samples were 97.9%-104.7% and 93.4%-100.0%, respectively, with relative standard deviations （RSDs） of 1.34%-2.43%. The method was simple, rapid, precisive, accurate, and solvent saving, suitable for batch testing .
Keywords： solanesol； extraction； saponification； ultra performance liquid chromatography
茄尼醇（Solanesol）是一种植物叶片中普遍存在的C45聚戊二烯醇,烟草是茄尼醇含量最丰富的植物,其含量可达4%[1-2].茄尼醇不仅是影响烟草香吃味和安全性品质的重要化学成分[3],也是合成治疗心血管疾病及抗癌、抗溃疡等新型药不可替代的中间体[2,4].由于茄尼醇分子量大,沸点高,液相色谱法是目前分离检测茄尼醇普遍采用的方法[5-16].茄尼醇在烟草体内以游离态和化合态两种形式存在,化合态茄尼醇需经过皂化反应变成游离态才能通过液相色谱分离检测.据资料报道[6-10],烟草样品一般在水浴条件下,经过复杂的提取、皂化、液液分配、柱层析、浓缩等程序,获得总茄尼醇待测液,样品前处理耗时长,溶剂消耗量大.Chen等[11]、Zhou等[12]分别研究了微波辅助提取、皂化烟草总茄尼醇的方法,该方法虽然步骤简单,但溶剂消耗量较大,且不利于批量操作.潘葳等[13]、赵春建等[14]、Mahendra等[15]、张婕等[16]分别研究发现,超声波辅助提取烟叶游离茄尼醇,具有时间短,溶剂用量少,提取温度低,操作简单等优点.但目前还未见超声波辅助提取同时皂化烟草结合态茄尼醇从而获得总茄尼醇的研究报道.为简化烟草总茄尼醇提取、皂化方法,提高检测效率,减少溶剂消耗,本文进行了超声波辅助条件下同时提取、皂化,并用高效液相色谱法检测烟草总茄尼醇的技术研究.
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结论：茄尼醇同步提取皂化—超高效液相色谱测定方法为关于对写作高效液相色谱论文范文与课题研究的大学硕士、相关本科毕业论文高效液相色谱图怎么看论文开题报告范文和相关文献综述及职称论文参考文献资料下载有帮助。
