山西老陈醋醋龄拉曼光谱快速检测方法的建立
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摘要
该文建立了山西老陈醋醋龄拉曼光谱快速检测方法。首先确定川穹嗪的拉曼特征峰,其次,对山西老陈醋川芎嗪纳米增强拉曼光谱快速检测方法积分时间、积分次数、平滑系数、检测功率、样品量进行优化,从精密度、重复性、加标回收率3个方面进行方法学评价。最佳条件为:积分时间20 s,积分次数10次,平滑系数10,功率300 m W,样品量20μL。川穹嗪质量浓度在5～200 mg/m L与峰强具有较好的线性关系(R2=0. 925 1)。该方法精密度、重现性和准确度均较好,精密度在2. 3%～3. 6%,重复性在1. 6%～3. 2%,加标回收率在80. 5%～87. 2%。拉曼光谱快速检测方法能满足实验室及现场快速检测要求,实验结果可用于山西老陈醋醋龄的检测。
The aim of this study was to establish a rapid detection method to measure the age of Shanxi mature vinegar based on raman spectra. Firstly,the raman characteristic peak of ligustrazine was determined,followed by optimizing the integral time,integral number,smoothing coefficient,detection power,and sample amount of ligustrazine nano-enhanced raman spectroscopy. The results showed that the optimal working condition was as follows: integrated for 20 s for 10 times,the smoothing coefficient was 10,the power was 300 m W,and the sample volume was 20 μL.The concentration of ligustrazine had a good linear relationship( R2= 0. 9251) with peak intensity from 5 mg/m L to200 mg/m L. The precision( 2. 3%-3. 6%) and repeatability( 1. 6%-3. 2%) of the method were good,and the method was accurate as its recovery rate was 80. 5%-87. 2%. In conclusion,this detection method based on raman spectroscopy can meet the requirements of laboratory and on-site rapid detection,and the experimental results can be used for detecting the age of Shanxi mature vinegar.
The aim of this study was to establish a rapid detection method to measure the age of Shanxi mature vinegar based on raman spectra. Firstly,the raman characteristic peak of ligustrazine was determined,followed by optimizing the integral time,integral number,smoothing coefficient,detection power,and sample amount of ligustrazine nano-enhanced raman spectroscopy. The results showed that the optimal working condition was as follows: integrated for 20 s for 10 times,the smoothing coefficient was 10,the power was 300 m W,and the sample volume was 20 μL.The concentration of ligustrazine had a good linear relationship( R2= 0. 9251) with peak intensity from 5 mg/m L to200 mg/m L. The precision( 2. 3%-3. 6%) and repeatability( 1. 6%-3. 2%) of the method were good,and the method was accurate as its recovery rate was 80. 5%-87. 2%. In conclusion,this detection method based on raman spectroscopy can meet the requirements of laboratory and on-site rapid detection,and the experimental results can be used for detecting the age of Shanxi mature vinegar.
引文
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[21]郭培源,刘硕,杨昆程,等.色谱技术、光谱分析法和生物检测技术在食品安全检测方面的应用进展[J].食品安全质量检测学报,2015(8):3 217-3 223.
[22] MA W,CHEN W,QIAO R,et al. Rapid and sensitive detection of microcystin by immunosebsor based on nuclear magnetic resonance[J]. Biosensors and Bioelectronics,2009,25(1):240-243.
[23]史晓亚,高丽霞,李鑫,等.无损检测技术在食品安全快速筛查中的应用[J].食品安全质量检测学报,2017,8(3):747-753.
[24]中国国家标准化管理委员会.地理标志产品山西老陈:GB/T 19777—2013[S].
[25]武太鹏,马康.无损快速检测技术在生鲜食品品质鉴定中的应用[J].食品安全质量检测学报,2017,8(3):729-736.
[26]李鑫,黄登宇.追溯技术在食品追溯体系中的研究进展[J].食品安全质量检测学报,2017,8(5):1 903-1 908.
[2]杨文辉,龚国清,周怡,等.川芎嗪体内抗血栓活性及机制探究[J].中国临床药理学与治疗学,2012,17(3):241-245.
[3] CHEN J,TIAN J,GE H,et al. Effects of tetramethylpyrazine from Chinese black vinegar on antioxidant and hypolipidemia activities in Hep G2 cells[J]. Food&Chemical Toxicology,2017,109(11):930-940.
[4]王颖,李蕾,王兴达,等.川芎嗪代谢物糖酯衍生物的合成及生物活性[J].化学研究与应用,2018(1):41-45.
[5] FAN C,LIN X,WANG E. Clinicopathological significance of cathepsin D expression in non-small cell lung cancer is conditional on apoptosis-associated protein phenotype:an immunohistochemistry study[J]. Tumour Biology the Journal of the International Society for Oncodevelopmental Biology&Medicine,2012,33(4):1 045-1 052.
[6] MIMAE T,TSUTA K,MAESHIMA A M,et al. Cathepsin D as a potential prognostic marker for lung adenocarcinoma[J]. Pathology,Research and Practice,2012,208(9):534-540.
[7]郑春燕. COX-2介导川芎嗪抑制肺癌A549细胞侵袭转移的作用研究[D].济南:山东大学,2012.
[8] QIAN W,XIONG X,FANG Z,et al. Protective effect of tetramethylpyrazine on myocardial ischemia-reperfusion injury[J]. Evid Based Complement Alternat Med,2014(3):107 501.
[9]蒋跃绒,陈可冀.川芎嗪的心脑血管药理作用及临床应用研究进展[J].中国中西医结合杂志,2013,33(5):707-711.
[10]刘丹,戴丽蓉,刘纪宁.川芎嗪对免疫调节作用的研究进展[J].现代临床医学,2014,40(1):9-11.
[11]陈可冀.川芎嗪的化学、药理与临床作用[M].北京:人民卫生出版社,2014.
[12]贺鹏飞,李婷,彭晓光,等.山西老陈醋生产过程中川芎嗪含量变化规律的研究[J].食品工程,2011(2):54-56.
[13] CHEN J C,CHEN Q H,QIN G,et al. Simultaneous determination of acetoin and tetramethylpyrazine in traditional vinegars by HPLC method[J]. Food Chemistry,2010,122(4):1 247-1 252.
[14]李建龙,刘书亮,彭杨,等. HPLC法同时检测食醋中川芎嗪和阿魏酸的含量[J].食品工业科技,2015,36(9):287-291.
[15]张少飞,李婷,彭晓光,等.高效液相色谱法测定山西老陈醋中的川芎嗪[J].食品工程,2009(2):43-45.
[16]范鹏蒋林东,王小丹,等.紫外分光光度计与酶标仪测定盐酸川芎嗪含量的比较[J].西南国防医药,2010(7):720-722.
[17]陈松.壳聚糖在三种中草药提取液澄清中的应用研究[D].湛江:广东海洋大学,2015.
[18]吴红玲.吡嗪类化合物的合成及表征[D].西安:西北大学,2009.
[19]罗春,鲍时根.微波法合成1,3-二芳基吡嗪[1,2-a]苯并咪唑衍生物[J].实验室研究与探索,2013,32(9):38-42.
[20]陈恒杰,郭雷,方旺,等. 2,3-二氯吡嗪的红外、拉曼光谱和密度泛函研究[J].光谱学与光谱分析,2014(11):2 994-2 998.
[21]郭培源,刘硕,杨昆程,等.色谱技术、光谱分析法和生物检测技术在食品安全检测方面的应用进展[J].食品安全质量检测学报,2015(8):3 217-3 223.
[22] MA W,CHEN W,QIAO R,et al. Rapid and sensitive detection of microcystin by immunosebsor based on nuclear magnetic resonance[J]. Biosensors and Bioelectronics,2009,25(1):240-243.
[23]史晓亚,高丽霞,李鑫,等.无损检测技术在食品安全快速筛查中的应用[J].食品安全质量检测学报,2017,8(3):747-753.
[24]中国国家标准化管理委员会.地理标志产品山西老陈:GB/T 19777—2013[S].
[25]武太鹏,马康.无损快速检测技术在生鲜食品品质鉴定中的应用[J].食品安全质量检测学报,2017,8(3):729-736.
[26]李鑫,黄登宇.追溯技术在食品追溯体系中的研究进展[J].食品安全质量检测学报,2017,8(5):1 903-1 908.