1 河南工业大学粮油食品学院, 河南 郑州 450001
2 中国科学院重庆绿色智能技术研究院, 太赫兹技术研究中心, 跨尺度制造技术重庆市重点实验室, 重庆 400714
3 内蒙古农业大学生命科学学院, 内蒙古 呼和浩特 010018
4 中国科学院重庆绿色智能技术研究院, 单分子精准医疗研究中心, 跨尺度制造技术重庆市重点实验室, 重庆 400714
研究太赫兹时域光谱(Terahertz Time-domain Spectroscopy, THz-TDS)技术和红外光谱技术用于硫酸软骨素掺假鉴定的可行性. 将六偏磷酸钠混入鲨鱼硫酸软骨素中的样品作为掺假研究对象, 利用上述两种技术对样品进行对比研究. 研究发现, THz光谱和红外光谱谱图中六偏磷酸钠标样、鲨鱼硫酸软骨素标样与掺假(混合)样品谱线均表现出较明显的差异, 可用于鉴别鲨鱼硫酸软骨素的六偏磷酸钠掺假. 实验结果表明, 此两种技术能够鉴别的六偏磷酸钠: 鲨鱼硫酸软骨素最低质量比分别为1: 15和1: 1, THz-TDS表现出较为灵敏的检测性能; 综合考虑, THz-TDS技术可以比较好的用于鲨鱼硫酸软骨素的六偏磷酸钠掺假检测. 本工作为发展一种基于THz-TDS技术的准确、快速和无损鉴别鲨鱼硫酸软骨素掺假的新型光谱技术奠定了前期实验基础.
光谱检测 硫酸软骨素 六偏磷酸钠 食品掺假鉴定 spectroscopic detection chondroitin sulfate sodium hexametaphosphate food adulteration inspection
厦门大学医学院抗癌研究中心, 福建 厦门 361102
硫酸软骨素的测定在生物医学领域有重要价值,但常规检测法在灵敏度、选择性或简易性方面尚存在不足.本文基于带正电基团的阳离子表面活性剂对具有红区发射特性的强荧光化合物—荷负电的四磺基铝酞菁具有高效荧光猝灭作用,而在生物多糖硫酸软骨素存在下,上述荧光猝灭体系荧光显著恢复的现象,提出酞菁-表面活性剂离子缔合物荧光恢复高灵敏测定硫酸软骨素的新方法,并用于实际样品分析.研究表明,中性介质中,红区荧光探针四磺基铝酞菁(Tetrasulfonated aluminium phthalocyanine,AlS4Pc)与阳离子表面活性剂十四烷基二甲基苄基氯化铵(Tetradecyldimethylbenzylammonium chloride,TDBAC)发生强烈的缔合作用,导致AlS4Pc的荧光几乎完全猝灭,从而获得暗背景的荧光体系.在加入带有阴离子基团(磺酸基)的生物多糖硫酸软骨素(Chondroitin sulfate,CS)后,由于竞争结合作用,AlS4Pc被释放而使体系的荧光大幅度恢复,且恢复程度与CS呈线性正相关.优化了反应条件,考察了共存物质的影响,结果表明本法具有较好的选择性.在最佳条件下,线性范围为0.20~10.0 μg·mL-1,检测限为0.070 μg·mL-1,工作曲线方程y=1.04x+2.09,r=0.999 5.该法操作简便,灵敏度、稳定性与准确性好,实际样品的分析结果令人满意.酞菁荧光化合物在分析科学中的应用尚不多见,本文工作进一步开拓了酞菁红区荧光探针的新应用.
硫酸软骨素 酞菁 荧光 测定 Fluorescence Phthalocyanine Chondroitin sulfate Determination 光谱学与光谱分析
2015, 35(8): 2203
Author Affiliations
Abstract
1 School of Pharmaceutical Sciences and National Glycoengineering Research Center Shandong University, No. 44 Wenhuaxi Road Jinan 250012, P. R. China
2 School of Chemistry and Chemical Engineering Shandong University, No. 27 Shandanan Road Jinan 250010, P. R. China
Near infrared spectroscopy (NIRS) is based on molecular overtone and combination vibrations. It is difficult to assign specific features under complicated system. So it is necessary to find the relevance between NIRS and target compound. For this purpose, the chondroitin sulfate (CS) ethanol precipitation process was selected as the research model, and 90 samples of 5 different batches were collected and the content of CS was determined by modified carbazole method. The relevance between NIRS and CS was studied throughout optical pathlength, pretreatment methods and variables selection methods. In conclusion, the first derivative with Savitzky–Golay (SG) smoothing was selected as the best pretreatment, and the best spectral region was selected using interval partial least squares (iPLS) method under 1mm optical cell. A multivariate calibration model was established using PLS algorithm for determining the content of CS, and the root mean square error of prediction (RMSEP) is 3.934 g·L-1. This method will have great potential in process analytical technology in the future.
Chondroitin sulfate near infrared spectroscopy variable selection pathlength Journal of Innovative Optical Health Sciences
2014, 7(6): 1450022
