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1、工学硕士学位论文气相色谱-质谱联用法分析酒中塑化剂和香气成分哈尔滨理工大学2014年3月国内图书分类号：X524工学硕士学位论文气相色谱-质谱联用法分析酒中塑化剂和香气成分硕 士 研究生：导 师：申请学位级别：工学硕士学 科、专 业：应用化学所 在 单 位：化学与环境工程学院答 辩 日 期：2014年3月授予学位单位：哈尔滨理工大学Classified Index：X524Dissertation for the Master Degree in EngineeringStudy on the analysis of plasticizer and aroma components in wi
2、ne by gas chromatography-mass spectrometryCandidate： Supervisor： Academic Degree Applied for： Master of EngineeringSpecialty： Applied ChemistryDate of Oral Examination： March, 2014University： Harbin University of Science and Technology哈尔滨理工大学硕士学位论文原创性声明本人郑重声明：此处所提交的硕士学位论文产氢菌培养条件的优化及脱氢酶活性的测定条件研究，是本人在
3、导师指导下，在哈尔滨理工大学攻读硕士学位期间独立进行研究工作所取得的成果。据本人所知，论文中除已注明部分外不包含他人已发表或撰写过的研究成果。对本文研究工作做出贡献的个人和集体，均已在文中以明确方式注明。本声明的法律结果将完全由本人承担。 作者签名： 日期： 年 月 日哈尔滨理工大学硕士学位论文使用授权书产氢菌培养条件的优化及脱氢酶活性的测定条件研究系本人在哈尔滨理工大学攻读硕士学位期间在导师指导下完成的硕士学位论文。本论文的研究成果归哈尔滨理工大学所有，本论文的研究内容不得以其它单位的名义发表。本人完全了解哈尔滨理工大学关于保存、使用学位论文的规定，同意学校保留并向有关部门提交论文和电子版本
4、，允许论文被查阅和借阅。本人授权哈尔滨理工大学可以采用影印、缩印或其他复制手段保存论文，可以公布论文的全部或部分内容。本学位论文属于 保密 在 年解密后适用授权书。 不保密 (请在以上相应方框内打)作者签名： 日期： 年 月 日导师签名： 日期： 年 月 日哈尔滨理工大学工学硕士学位论文气相色谱-质谱联用法分析酒中塑化剂和香气成分摘 要酒是餐桌上不可或缺的饮品。近几年，随着假、劣质酒在市场中频繁出现，酒中毒事故时有发生，严重威胁到人们的身心健康，酒质量控制成为普通百姓关心的焦点问题。目前，塑化剂分析和香气成分鉴定是酒质量检测技术领域的研究热点，其重要性愈加受到人们的广泛关注。本论文以气相色谱-
5、质谱联用技术为检测手段，以溶剂萃取和固相萃取为样品前处理方法，将邻苯二甲酸酯(Phthalate esters, PAEs)和香气成分作为分析目标，建立了酒中塑化剂检测和香气成分鉴定方法。(1) 以北大仓白酒为检测样本，建立了15种邻苯二甲酸酯类物质的气相色谱-质谱联用定性和定量分析方法。在样品前处理技术上，考察了2种不同萃取方式中4种不同溶剂和2种不同填料对目标物质的吸附能力；在分离方式上，依据沸点和极性参数，采用毛细管柱程序升温技术实现了15种化合物的良好分离；在定性和定量方法上，以保留时间加特征选择离子为定性参数，选择离子质量峰面积为定量参数，保证了对目标化合物定性和定量的准确性。在精密
6、度和准确度两方面对所建立的方法进行了有效性验证，并将该方法用于北大仓白酒实际样品的检测。(2) 以北大仓白酒为检测样本，建立了其香气成分的气相色谱-质谱联用分析方法。比较了溶剂萃取和固相萃取两种方法对目标香气成分的提取能力，从二氯甲烷提取物中分离并鉴定了30种香气成分物质，从而构建了北大仓白酒香气成分的“骨架”。(3) 以忠芝蓝莓酒为检测样本，建立了其香气成分的气相色谱-质谱联用分析方法。比较了溶剂萃取和固相萃取两种方法对目标香气成分的提取能力，从二氯甲烷提取物中分离并鉴定了52种香气成分物质，从而构建了忠芝蓝莓酒香气成分的“骨架”。关键词 北大仓白酒；忠芝蓝莓酒；塑化剂；香气成分；气相色谱-
7、质谱Study on the analysis of plasticizer and aroma components in wine by gas chromatography-mass spectrometryAbstractWine is a kind of indispensable drink on peoples dining-table. In recent years, with high frequency of adulterated and inferior wine in the market, wine poisoning accidents have often o
8、ccurred, which has endangered peoples health. Wine quality control has been the social focus. Nowadays, the analysis of plasticizer and aroma components is the hot research topic in the field of wine quality detecting technology, its importance has been paid a widespread attention. In this paper, us
9、ing GC-MS as detecting method, solvent and solid extraction as sample pretreatment method and phthalate esters and aroma components as analytical targets, the methods about plasticizer detection and aroma components identification in wine were developed. (1) Using BEIDACANG wine as detecting sample,
10、 a qualitative and quantitative GC-MS analytical method was developed for the analysis of phthalate esters. In the pre-concentration step, for two extraction forms，solvent extraction and solid phase extraction, the extraction capability of four different solvents and adsorbent performance of two typ
11、es of cartridges were investigated for 15 analytes; for the GC separation form, the good separation of 15 targets was achieved by using the temperature programmed technology of capillary column based on boiling point and polarity parameter; for the qualitative and the quantitative method, the retent
12、ion time and one or two characteristic ions of every analyte were choosed as qualitative parameters, peak area of extraction ion as quantitative parameters, the accurate determination of target compounds was ensured accordingly. The proposed method was validated for two aspects of accuracy and preci
13、sion and was used for the determination of real BEIDACANG wine sample. (2) Using BEIDACANG wine as detecting sample, a GC-MS method was developed for the analysis of its aroma components. The extraction performance of two means, solvent extraction and solid phase extraction, was compared for the tar
14、get aroma components. For all separated peaks obtained from dichloromethane extract of BEIDACANG wine, 30 aromatic substances were identified, accordingly, the “skeleton” of aroma component in BEIDACANG wine was confirmed. (3) Using ZHONGZHI blueberry wine as detecting sample, a GC-MS method was dev
15、eloped for the analysis of its aroma components. The extraction performance of two means, solvent extraction and solid phase extraction, was compared for the target aroma components. For all separated peaks obtained from dichloromethane extract of ZHONGZHI blueberry wine, 52 aromatic substances were identified, accordingly, the “skeleton” of aroma component in ZHONGZHI blueberr
