Microsoft Word 叶少文_二校出4189

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1 7 10 Vol. 7 No Journal of Food Safety and Quality Oct., 2016 * 叶少文 (, ) 摘要 : 目的 (2015 ), 方法,,,, 结果 0.054~0.648 mg/ml, r> % 98.10% 98.68% 结论,, 关键词 : ; ; ; Optimization of the extraction and detection method of mannose in Dendrobium officinale Kimuraet Migo YE Shao-Wen * (By-HeaLth Co., Ltd., Zhuhai , China) ABSTRACT: Objective To discuss the detection method of mannose in Dendrobium officinale Kimuraet Migo in harmacopoeia of People s Republic of China Part I (2005 Edition) and simplify the operation steps of existing method. Methods The free monosaccharide in Dendrobium officinale Kimuraet Migo samples was removed by ultrasonic extraction method instead of soxhlet extraction, and the mannose in samples was extracted by microwave method instead of dew decoction method. There was no derivative reaction and internal standard method in this method. The sample extract was filtered by microporous filtering film, then analyzed by the high performance liquid chromatography (HPLC) described in harmacopoeia, and the content of mannose was determined by external standard method. Results There was a good linear relationship between the mannose content which ranged from 0.054~0.648 mg/ml and peak area with the correlation coefficient (r) greater than The average recoveries of mannose at 3 different adding levels were 97.66%, 98.10% and 98.68%, respectively. Conclusion This method is simple, accurate, precise, and greatly shorten the processing time, which can be used to the content determination of mannose in Dendrobium officinale Kimuraet Migo. KEY WORDS: Dendrobium officinale Kimuraet Migo; mannose; microwave extraction; high performance liquid chromatography * 通讯作者 :,, @qq.com *Corresponding author: YE Shao-Wen, Licensed Pharmacist, By-Health Co., Ltd, Zhuhai , China @qq.com

2 引言 (Dendrobium officinale Kimuraet Migo),,,, [1],, [2], [3] (2015 ) [4],,, [5],, [6] 2 材料与方法 2.1 试剂和仪器 ( 100%, ); ; (, ); (, ); ( ) Waters e2695 (, Waters ) 2.2 实验方法液相色谱条件 : Rezex RCM-Monosaccharide Ca 2+ (300mm 7.8 mm) Ca 2+ [7] ; : 65 ; : 65 ;, : 0.4 ml/min; : 40 μl; : 40 min [8] 标准曲线的绘制 : 50 mg, 10 ml, 5.0 mg/ml, ml 10 ml, mg/ml 0.45 μm,,, (X), (Y), [8] 样品供试液的配制 ( ) ( 0.1 g, 0.15 mg/ml ) 250 ml, 80 % 150 ml, 20 min;, ; 30 ml, (400 W) 5 min; 50 ml, 8000 r/min 5 min, 5 ml 25 ml, 1.5 ml 12%,, min;, 10 % ph (ph ), 25 ml,, 0.45 μm, [9] (2015 ) 精密度实验 6, 2.2.3,, (relative standard deviation, RSD) [10] 加标回收实验 9 ( ) ( 0.10 mg/ml ) 50 ml, 3, 3, mg (, 40% 50% 60% ), 30 ml, (400 W) 5 min; 50 ml, 8000 r/min 5 min, 5 ml 25 ml, 1.5 ml 12%,, min;, 10 % ph (ph ), 25 ml,, 0.45 μm,, [11] 3 结果与分析 3.1 甘露糖的标准曲线 1, Y=852119X , r=0.9999, 0.054~0.648 mg/ml [12] 1 Fig. 1 Standard curve of mannose

3 10 : 检出限和定量限 (limit of detection, LOD) (limit of quantification, LOQ) (S/N) LOD S/N=3, LOQ S/N=10 [13] 检出限 0.15 μg/ml, S/N=3, : 0.15 μg/ml 150 ml/1000/100 mg 100%=0.0225% 定量限 LOD LOQ, LOQ LOD/3 10,, : %/3 10=0.075% 3.3 精密度实验 % 22.36% 22.24% 22.40% 22.31% 22.25%, RSD 1.3%, [14] 3.4 加标回收实验 3 1, 1, % 98.10% 98.68%, RSD 0.5% 0.5% 1.2% [15] 3.5 样品测定实际样品测定 2 3,,, (2015 ), 2, 2 2 (mg) 表 1 Table 1 (mg) 加标回收率实验结果 The results of recoveries 讨论与结论 (%) (%) RSD(%) (2015 ),,, ,,,,, :,, 2 Fig. 2 Chromatogram of sample

4 Fig. 3 Chromatogram of mannose standard 表 2 甘露糖含量测定结果比较 Table 2 The comparison of mannose contents (%) (%) RSD(%) (2015 ) (%) (%) RSD(%) , 2,, 320 min, 80 min,, 参考文献 [1],. [J]., 2011, 21(4): Qian GM, Zhang HP. Research progress of the chemical components and pharmacological activity of Gold hair pin caulis dendrobii [J]. Chin Med Mod Dist Educ China, 2011, 21(4): [2],,,. [J]., 2011, 14(1): Wang WY, Zou H, Chen YK, et al. Comprehensive utilization and prospect of Dendrobium officinale Kimuraet Migo [J]. Chin Hortic Abstr, 2011, 14(1): [3],. [J]., 2013, 10(7): Gao XJ, Wang CS. Application of fresh Dendrobium officinale Kimuraet Migo [J]. Beijing J Tradit Chin Med, 2013, 10(7): [4]. (2015 ) [M]. :, National Pharmacopoeia Committee. Pharmacopoeia of People s Republic of China Part I (2005 Edition) [M]. Beijing: Chemical Industry Pres s, [5],,,. [J]., 2004, 15(4): Yang H, Wang SC, Wang ZT, et al. The research of mannose in Dendrobium officinale Kimuraet Migo [J]. Chin Pharm J, 2004, 15(4): [6],. [J]., 2001, 02(1): Chen XM, Guo SX. Research progress of chemical composition and pharmacological activity of plants belong to Dendrobium Sw. [J]. Nat Prod Res Dev, 2001, 02(1): [7],,. [J].,

10 : 4191 2001, 11(2): 43 45. Wang J, Wang Q, Xiang WS. Application of chromatography in the analysis of carbohydrate compounds [J]. Chin J Anal Chem, 2001, 11(2): 43 45. [8],,,. [J]., 1994, 05(3): 72 75.

5 10 : , 11(2): Wang J, Wang Q, Xiang WS. Application of chromatography in the analysis of carbohydrate compounds [J]. Chin J Anal Chem, 2001, 11(2): [8],,,. [J]., 1994, 05(3): Huang MQ, Huang BH, Cai TY, et al. Extraction, separation and analysis of mannose in Dendrobium officinale Kimuraet Migo [J]. Chin Tradit Herb Drugs, 1994, 05(3): [9]. [J]., 2010, 22(18): Shang XY. Comparative study on the extraction of polysaccharide from Dendrobium officinale Kimuraet Migo using water extraction method and enzyme method [J]. Anhui Agric Sci, 2010, 22(18): [10], 乂,. [J] ,10(18):52-53 Liu HL, Shang ZY, Qu WL. Tin caulis dendrobii health products research and development value [J]. Journal of China national folk medicine (18), [11],,. [J] ,05(06)11-13 Lv JN, Chen SH, Xu JH. Caulis dendrobii polysaccharide of Tin caulis dendrobii root s extraction of the response surface method optimization study [J]. Journal of zhejiang of traditional Chinese medicine, 2014,05 (06)11-13 [12],,. [J] ,11(05)42-44 amino acids and alkaloid content in caulis dendrobii comparison [J]. Journal of traditional Chinese medicine. 2014,11 (05)42-44 [13],. [J] ,02(23) Nie SP, Cai HL. Tin caulis dendrobii active ingredient and its research progress function [J]. Journal of food science. 2012,02 (23)75-77 [14],,. [J] ,06(12) Gu HF, Xin XJ, Zhou WT Etc. Tin caulis dendrobii tube seedlings growth and cultivation research and polysaccharide content determination [J]. Proprietary of Chinese medicine. 1999,06(12)18-20 [15],,. [J] ,12(05)21-23 He TG, Yang LT, Li YR Etc. Tin caulis dendrobii protocorm polysaccharide extract optimum technological research [J]. Journal of northwest agriculture. 2006,12 (05)18-20 作者简介 ( 责任编辑 : 刘丹 ) 叶少文, 执业药师, 主要研究方向为保健食品的质量检测 @qq.com Wang QH, He XJ, Bao ZB Etc. Different sources of iron polysaccharides,

Microsoft Word 叶少文-二校-出3129、3130、3131、3132

Microsoft Word 叶少文-二校-出3129、3130、3131、3132 6 8 Vol. 6 No. 8 2015 8 Journal of Food Safety and Quality Aug., 2015 L- * 叶少文 (, 519040) 摘要 : 目的, L-, L- 方法,,, Na, L- 结果 L- 0.3861~3.0648 mg/ml, r>0.999 80% 100% 120%, L- 97.2% 结论, L- 关键词 : ; ; L- Determination

Microsoft Word 叶少文_二校 出4189

Microsoft Word 叶少文_二校出4189