齐齐哈尔大学学报（自然科学版）
齊齊哈爾大學學報（自然科學版）
제제합이대학학보（자연과학판）
JOURNAL OF QIQIHAR UNIVERSITY(NATURAL SCIENCE EDITION)
2014年
3期
19-22,26
,共5页
残留溶剂%固相微萃取%聚酰亚胺硅氧烷%气相色谱
殘留溶劑%固相微萃取%聚酰亞胺硅氧烷%氣相色譜
잔류용제%고상미췌취%취선아알규양완%기상색보
residual solvents%solid phase microextraction%polyimide siloxane%gas chromatography
将4,4′-二氨基二苯醚（ODA）、均苯四甲酸二酐（PMDA）和1,3-双（3-氨基丙基）-1,1,3,3-四甲基二硅氧烷进行共聚反应，得到含硅聚酰胺酸（PAA）。经高温脱水环化，含硅聚酰胺酸中氨基与石英纤维表面羟基脱水缩合，键合到石英纤维表面，制备了聚酰亚胺硅氧烷固相微萃取头。通过红外光谱、热重分析、扫描电镜、X射线光电子能谱对涂层的性能进行表征。采用顶空固相微萃取--气相色谱法对盐酸丙帕他莫、加替沙星、盐酸托莫西汀、沙美特罗、吡哌酸、替莫唑中间二甲苯、二甲基亚砜、硝基苯3种残留溶剂进行分析，间二甲苯在0.17～6.88μg/mL、二甲基亚砜在0.22～8.80μg/mL、硝基苯在0.24～9.60μg/mL浓度范围内呈良好的线性关系，线性相关系数（r）分别为0.9917，0.9972和0.9915，最低检测限分别为0.029，0.036，0.059μg/mL，相对标准偏差（n=6）分别为2.07%，3.56%，2.94%。
將4,4′-二氨基二苯醚（ODA）、均苯四甲痠二酐（PMDA）和1,3-雙（3-氨基丙基）-1,1,3,3-四甲基二硅氧烷進行共聚反應，得到含硅聚酰胺痠（PAA）。經高溫脫水環化，含硅聚酰胺痠中氨基與石英纖維錶麵羥基脫水縮閤，鍵閤到石英纖維錶麵，製備瞭聚酰亞胺硅氧烷固相微萃取頭。通過紅外光譜、熱重分析、掃描電鏡、X射線光電子能譜對塗層的性能進行錶徵。採用頂空固相微萃取--氣相色譜法對鹽痠丙帕他莫、加替沙星、鹽痠託莫西汀、沙美特囉、吡哌痠、替莫唑中間二甲苯、二甲基亞砜、硝基苯3種殘留溶劑進行分析，間二甲苯在0.17～6.88μg/mL、二甲基亞砜在0.22～8.80μg/mL、硝基苯在0.24～9.60μg/mL濃度範圍內呈良好的線性關繫，線性相關繫數（r）分彆為0.9917，0.9972和0.9915，最低檢測限分彆為0.029，0.036，0.059μg/mL，相對標準偏差（n=6）分彆為2.07%，3.56%，2.94%。
장4,4′-이안기이분미（ODA）、균분사갑산이항（PMDA）화1,3-쌍（3-안기병기）-1,1,3,3-사갑기이규양완진행공취반응，득도함규취선알산（PAA）。경고온탈수배화，함규취선알산중안기여석영섬유표면간기탈수축합，건합도석영섬유표면，제비료취선아알규양완고상미췌취두。통과홍외광보、열중분석、소묘전경、X사선광전자능보대도층적성능진행표정。채용정공고상미췌취--기상색보법대염산병파타막、가체사성、염산탁막서정、사미특라、필고산、체막서중간이갑분、이갑기아풍、초기분3충잔류용제진행분석，간이갑분재0.17～6.88μg/mL、이갑기아풍재0.22～8.80μg/mL、초기분재0.24～9.60μg/mL농도범위내정량호적선성관계，선성상관계수（r）분별위0.9917，0.9972화0.9915，최저검측한분별위0.029，0.036，0.059μg/mL，상대표준편차（n=6）분별위2.07%，3.56%，2.94%。
Silicon-containing polyimide acid(PAA)was synthesized from 4,4'-diaminodiphenylether(ODA), pyromellitic acid dianhydride(PMDA)and 1,3-bis(3-aminopropyl)tetramethyldisiloxane. The coating were bonded on the quartz fiber surface by the condensation reaction between the polymeride and the silicon alcohol. The polyimide siloxane solid-phase microextraction head were prepared.The performance of the coating was characterized by IR,thermal analysis,scanning electron microscope,X-ray photoelectron spectroscopy.Dimethyl sulfoxide,and in PorpacetamolHydrgqhloride,gatifloxacin,atomoxetine hydrochloride,salmeterol,pipemidic acid, temozolomide were detected by head space-solid phase microextraction-gas chromatography.The linear relationship were obtained in the ranges of 22.0-132μg/mL(for dimethyl sulfoxide),8.60-51.6μg/mL(for m-xylene), 24.0-144μg/mL(for nitrobenzene).The correlation coefficients(r)were 0.9972, 0.9917 and 0.9915 respectively. The lowest detection limits were 3.7μg /mL,2.9μg/mLand 3.4μg/mL. The relative standard deviations were 3.56%, 2.07%and2.94% (n=6) repectively.
