臺灣大學: 化學研究所何國榮黃珮嘉Huang, Pei-ChiaPei-ChiaHuang2013-04-112018-07-102013-04-112018-07-102011http://ntur.lib.ntu.edu.tw//handle/246246/257300　　氨基甲酸酯類和尿素類農藥因不易帶電，所以大部分文獻常以微胞電層析分離此類中性分析物。然而，當銜接微胞電層析至電灑質譜時，界面活性劑會影響分析物的靈敏度和汙染質譜的離子源。本實驗利用低流速鞘流-液體結合式介面，成功銜接微胞電層析至質譜，藉由控制銜接管的電滲流至小於微胞回退的速度，減少微胞引入質譜而提升農藥分析物的訊號強度(約2~10倍)。搭配質譜/質譜的偵測模式，可成功分離並偵測到十九種農藥分析物。在定量方面，以carbofuran(19種農藥之一)做初步評估，在濃度0.05 ppm到10 ppm間與層析峰面積有很好的線性關係，因此此方法亦具有定量的潛力。 　　本實驗亦利用低流速鞘流-液體結合式介面結合微胞電層析與毛細管區帶電泳，在第一段分離使用微胞電層析，第二段的分離則使用區帶電泳，藉由結合兩種不同的分離機制而增加分離解析度。以磺胺類藥物為例，在pH 5.5時，使用適當的毛細管長度與電場結合微胞電層析與區帶電泳，可使原本在微胞電層析中重疊的SMP(5)和SMP(7)因第二段區帶電泳得到有效分離，而在區帶電泳中淌度相近的SMR(2)、STZ(3)、SMP(5)和SMZ(6)也可藉由第一段的微胞電層析改善分離效果。因此在合適的條件下結合此兩種分離機制，可改善在單一分離機制中重疊分析物之分離，提升分離效果。Because carbamate and urea-type pesticides are netural at wide pH range, MEKC was often used to separate these netural compounds. However, nonvolatile surfactants in MEKC would decrease the sensitiveity of analytes on MS and contaminate the ion source of MS. A liquid-junction/low-flow interface was utilized to reduce the introduction of micelle into ESI source by controlling the EOF of connecting capillary. The signal intensity of pesticide analytes were enhanced about 2-10 fold. With MS/MS detection, 19 pesticide analytes were sucessfully separated and detected. Moreover, carbofuran(one of 19 pesticides) was used to evaluate the quantitative ability of this method. The result showed that a relationship between peak area of EIC and concentration is linear in the range 0.05ppm to 10ppm. 　 To enhance the separation, a liquid-junction/low-flow interface was utilized to combine MEKC with CZE. The MEKC-CZE method was used for sulfonamide analysis at pH 5.5. With appropriate capillary length (MEKC :CZE=4 :1) and electric field, SMP(5) and SMP(7), which were overlapped in MEKC, were separated in MEKC-CZE. In addition, SMR(2)、STZ(3)、SMP(5) and SMZ(6), which were coeluted in CZE, were also resolved in MEKC-CZE. Therefore, combining these two techniques by proper conditions would improve separation of coeluent in single separation mechanism.3639821 bytesapplication/pdfen-US微胞電層析電灑法質譜氨基甲酸酯類和尿素類農藥質譜/質譜微胞電層析結合毛細管區帶電泳磺胺類藥物MEKC-ESI/MScarbamate and urea-type pesticidesMS/MSMEKC-CZEsulfonamidesthesishttp://ntur.lib.ntu.edu.tw/bitstream/246246/257300/1/ntu-100-R98223104-1.pdf