Determination of the Degree of Deacetylation of Chitinous Materials by Near-Infrared Spectroscopy
Date Issued
2004
Date
2004
Author(s)
Tsai, Chih-Cheng
DOI
zh-TW
Abstract
本研究以近紅外光技術探討幾丁質（Chitin）在製備幾丁聚醣（Chitosan）的去乙醯化製程中，各階段之不同形態下的光譜分析，包括粉末形態（幾丁質去乙醯化前的混合粉末）、去乙醯過程溶液（幾丁質去乙醯化反應中）、去乙醯化後幾丁聚醣粉末、以及和尚蟹膜之去乙醯率（DD）檢測應用。
以幾丁質混合粉末模擬不同去乙醯率之樣本，在MLR模式分析所挑選的重要分析波長為1528，1592，1662，1692，2022及2102 nm。去乙醯反應後之粉末樣本的MLR檢量線分析結果，以二次微分的六波長組合（898，1402，2310，428，1990及2016 nm）為最佳，rc=0.996，SEC=0.013，RSEC=1.0%，rp=0.996，SEP=0.015，RSEP=1.3%，RPD=13.8。在粉末幾丁類物質產品的近紅外光去乙醯率測定，此為最佳之檢量線預測模式。
幾丁質在去乙醯化過程中，即時量測懸浮液樣本光譜的分析結果，在使用部份特徵波段600∼1000 nm與1400∼1500 nm之二次微分光譜MPLSR分析，可得最佳光譜檢量線，其rc=0.991，SEC=0.019，RSEC=1.4%， rp=0.990，SEP=0.022，RSEP=3.4%，RPD=9.4，此模式可作為幾丁質製備幾丁聚醣即時線上檢測及品質監控之應用。
去乙醯和尚蟹皮膜的分析結果在濕膜的最佳檢量線為全波段（400∼2500 nm）光譜之二次微分的MPLSR分析結果，rc=0.885，SEC=0.065，rp=0.800，SEP=0.076。去乙醯和尚蟹皮膜之乾膜分析結果以MPLSR全波段二次微分rc=0.932，SEC=0.052，rp=0.921，SEP=0.056為預測去乙醯率之最佳檢量線模式。從廢棄蟹殼純化出幾丁質與幾丁聚醣，並應用近紅外光技術快速檢測其去乙醯率，在水產資源的利用層面而言是非常有價值的。
本研究已成功的建立幾丁類物質之去乙醯率檢測模式，包括幾丁質與幾丁聚醣粉末之去乙醯率近紅外光檢測模式、幾丁質在製備幾丁聚醣的去乙醯化過程中，樣本即時檢測去乙醯率的近紅外光檢測模式，以及去乙醯和尚蟹皮膜濕膜與乾膜去乙醯率檢量線的建立。
This study is aimed to investigate the degree of deacetylation（DD）measurements of chitinous materials in powder, suspension liquid and membrane forms using near infrared（NIR）spectroscopy.
The spectrum analysis of the chitin and chitosan powder mixture exhibited absortion wavelengths at 1528, 1592, 1662, 1692, 2022 and 2102 nm by MLR（Multiple Leaner Regression）model. The best results of deacetylated chitinous powder from suspension liquid were given by MLR with six wavelengths combination ( 898, 1402, 2310, 428, 1990 and 2016 nm ) with the second derivative treatment, which were rc=0.993, SEC=0.013, RESC=1.0%, rp=0.996, SEP=0.015, RSEP=1.3%, RPD=13.8. For the determination of the degree of deacetylation.
During the process of the deacetylation, the real-time measurement of suspension was adoped. The MPLSR（Modified Partial Least Squares Regression）model with second derivative spectra in the range of 600~1000 and 1400~1500 nm yielded the best results, which were rc=0.991, SEC=0.019, RESC=1.4%, rp=0.990, SEP=0.022, RSEP=3.4%, RPD=9.4. This model could be used for real-time and on-line DD determination in preparing chitosan from suspension.
The degree of deacetylation calibration model of the Mictyris brevidactylus membrane was MPLSR method with second derivative spectra in the range of 400~2500 nm, and its results are rc=0.885, SEC=0.065, rp=0.800, SEP=0.076 for wet membrane; while rc=0.932, SEC=0.052, rp=0.921, SEP=0.056 for dried membrane. The application of NIR to DD measurements has importance to convert chitinous materials from crab shell which is regarded as waste.
This study had successfully developed the models for chitinous DD determination using NIR Spectroscopy, including DD determination model for chitin and chitosan powder, the real-time DD determination model for the chitinous suspension, and the DD determination model for Mictyris brevidactylus membrane in dried and wet state.
Subjects
近紅外光
去乙醯率
幾丁質
幾丁聚醣
Chitin
Chitosan
Degree of Deacetylation
Near-Infrared
Type
thesis
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