论文标题:UV固化固相微萃取新型涂层的开发和应用
The Development and Application of UV Curing Coating for SPME
论文作者 乔剑锋
论文导师 胡伟；李祖光,论文学位 硕士,论文专业 应用化学
论文单位 浙江工业大学,点击次数 81,论文页数 92页File Size4902k
2003-12-01论文网 http://www.lw23.com/lunwen_889666562/ 固相微萃取;紫外光固化;GC-MS
SPME,UV curing,GC-MS
本文首先对固相微萃取(SPME)技术进行了综述，对固相微萃取的过程参数优化研究，在样品预处理中的应用，研究展望，理论基础进行了介绍。本实验的工作包括以下几个方面： (1)用微量注射器组装法自制了简易固相微萃取装置，建立了评价SPME涂层富集能力的固体样品体系与液体样品体系。通过几种评价体系的比较，选择了具有溶液易于保存，分析速度较快，所用仪器要求较低等优点的标准溶液体系直接SPME方法作为主要评价体系，其他方法为辅助评价体系。 (2)对选择的直接SPME体系进行了分析测试条件优化，选择的组分为：三氯甲烷，乙酸，正戊醇，乙酸丁酯，N，N-二甲基甲酰胺，对二甲苯，环己酮，苯胺，苯酚。选择的色谱条件为：毛细管柱(UA-17-30m×0.25mm×0.25μm，50％-二苯基二甲基聚硅氧烷)，载气：N_2，0.1MP。氢火焰检测器：H_2，0.1MP；空气：0.1MP。不分流进样。柱温40℃保持1min，以8℃／min升至100℃保持2min。进样口温度220℃，检测器温度250℃。在此条件下，对各组分进行了方法的线性范围及检测限，方法的准确度，方法的精密度测定。(3)由常用的紫外光固化涂料原料开发了新型SPME涂层，提供了一种适合实验室自制SPME涂层的快捷方法。通过紫外光固化体系光敏齐聚物、活性稀释剂、添加剂主要组分的配方优化，开发了一种较好的配方。即以100％用量的助剂TF，AB及纳米MNIP0220为添加剂，100％浙江工业大学硕士学位论文 UV固化固相微萃取新型涂层的开发和应用用量的聚氨酷丙烯酸醋(基准)为主成分配制而成。 (4)用自制SPME装置的HS一SPME和常规HS方法进行了比较，在同样测定条件下，用自制的SPME装置对胡椒进行HS一SPME一GC一MS与常规HS方法进样10拼1进行比较，自制的SPME装置对某组分的响应峰面积为62052680，而进样10 pl对其组分的响应峰面积为38263，富集倍数为1622倍，说明自制SPME装置具有很强的富集能力。 (5)与国外SPME产品进行了比较，用自制的SPME装置(涂层体积仅为国外产品的涂层体积的1/4)和Supelc。公司的SPME(PA)，在同样分析条件下，对胡椒进行HS一SPME一GC一MS测定比较，由结果可知，对某些成分而言，自制SPME装置的吸附量比SUPELCO公司的SPME(PA)的吸附量至少高一倍。从总体上来看。自制SPME装置与 Supe1C。公司的SPME(PA)吸附富集能力基本相当。 (6)对直接SPME与直接进样进行了比较，本实验制得的SPME装置对对二甲苯的富集率为50.7，高于文献制备的SPME装置的富集率 10.7。 (7)用自制装置SPME一一GC/MS分别对山奈和新鲜的剑麻鲜花香气成分进行了剖析，效果令人满意，说明采用自制的SPME装置可成功地富集挥发性成分，可用于痕量挥发物的分析。
At first, this paper introduces solid phase microextraction ( SPME ) technology , includes studies of course parameter applications in the pretreatment of the sample, the prospect of study and the theoretical foundation,. Then, this paper introduces the work of this experiment including the following several respects:(1) Assemble a simple device for SPME with a micro- syringe, and set up the system for appraising the enrichment ability of SPME coating to solid sample and liquid sample. Through the comparison of several appraisal system, choose direct SPME method for main appraisal system because this system is relatively easy to be kept for standard solution, fast to be analysed and easy to get the instruments to use.(2) In order to optimize the condition of analysis for the chosen direct SPME system, the chosen components are: Chloroform, acetic acid, n-Amylalcohol, n-butyl acetate, DMF, p-xylene, cyclohexanone, aniline, Phenol. The chromatogram conditons chosen are: Column: (30m×0.25mm×0.25μm, UA-17), Carrier gas: N2, 0.1 MP. Detector:FID, H2,0.1MP; Air:0.1MP. split: off.Column temp : 40℃ (1 min ) to 100℃ (2 min) at 8℃ /min. Injector temp: 220℃, Detector temp:250℃. Under this condition, the linear range , the limits of detection , the recoveries, the relative standard deviations of the method to every component have been carried on.(3) Have been developed new-type SPME coating by the commonly used ultraviolet (uv) curing coating, has offered a kind of simple and convenient and fast method to be suitable for laboratory to make SPME coating by oneself . Through optimizing the liquid UV-curable composition (kind of oligomer, concentration of active diluent , photoinitiator and additive), we have got a kind of better ingredient , as follows: PUA 100% and additive (TF, AB and nanometer additive MNIP0220) 100%.(4) Compares HS-SPME (made of above ingredient) with routine HS method under the identic measuring condition. Take pepper for example, the area of responsing peak of main component is 62052680 in HS-SPME and 38263 in HS(10u1), a enrichment multiple of 1622, which is proved that this SPME coating has a better enrichment ability. (5) Compare self- SPME apparuts ( coating volume is only 1/4 offoreign products) with foreign SPME products - Supelco SPME( PA) , under the same analysing condition, earring on HS-SPME-GOMS for comparing, it can been seen by the result, as to some composition, the absorbing amount of self-SPME apparatus has at least one time higher than that of SPME( PA) of Supelco Company. Generally speaking, self-SPME apparatus and SPME( PA) of Supelco of Company have equal enrichment basically.(6) Compare direct SPME with direct inject, the SPME apparuts that is made by this experiment has the enrichment rate of 51 in P-Xylene, higher than the enrichment rate of SPME apparuts from the document.(7) Analyzed volatile chemical composition of two kind of herbs with HS-SPME" GC-MS. The results are satisfactory, proving that adopting self-SPME apparatus can be succeed in enrichment of volatility composition and used in the microanalysis of the volatile matter.
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