Microsoft Word 陈彩云-二校

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1 6 5 Vol. 6 No Journal of Food Safety and Quality May., 2015 陈彩云 *, 蔡伟江, 陈宏壁, 林贤邦 (, ) 摘要 : 目的, 方法, mol/l,, Diamonsil C 18, 192 nm 结果,, mg/ml~0.04 mg/ml, 1.000, 98.5%~100.0%, 0.6% 结论,,, 关键词 : ; ; ; Determination of chondroitin sulfate in health food by high performance liquid chromatography CHEN Cai-Yun *, CAI Wei-Jiang, CHEN Hong-Bi, LIN Xian-Bang (By-Health Co., Ltd., Zhuhai , China) ABSTRACT: Objective To investigate a quick and simple method for determination of chondroitin sulfate in health foods by high performance liquid chromatography (HPLC). Methods Samples were treated using mol/l pentane solution of sodium-acetonitrile as mobile phase with isocratic elution, separated on diamonsil C 18 column, and detected at 192 nm wavelength. Results Chondroitin sulfate could be separated well by this method. It had a good linear relationship within 0.008~0.04 mg/ml (r=1.000), the average recoveries was 98.5%~100.0%, and the RSD was 0.6%. Conclusion The method can be used for determination of chondroitin sulfate in health foods, it is quick, simple and accurate, and has a good reproducibility and clear separation, which can be popularized in the laboratory. KEY WORDS: high performance liquid chromatography; health foods; chondroitin sulfate; determination 1 引言,,,,,,, [1] : [2,3], [4], [5] [6-10],,,,, * 通讯作者 :, @qq.com *Corresponding author: CHEN Cai-Yun, By-Health Co., Ltd., Zhuhai , China @qq.com

2 ;,,,,,,,, ;,,,,, ;,,,,,,,,,,,,,,,, 2 材料与方法 2.1 仪器与试剂 ( 1260, ); (EQ-500, ); Diamonsil C 18 (250 mm 4.6 mm, 5.0μm, Dikma) ( : USP; : H1K241; : 100%); (, CNW); (, ); ; ( ) 2.2 仪器条件 : Diamonsil C 18 (250 mm 4.6 mm, 5.0μm, Dikma); : mol/l =5:95(v:v), ; : 0.8 ml/min; : 10 μl; : 192 nm [11] ; : 5 min 2.3 测定方法标准系列溶液的配制 mg, 50 ml, 5 ml, 10 min,,,, ml 25 ml,,, mg/ml, 0.45 μm C(mg/mL), (A), 供试品溶液配制 20,, 0.1 g, 50 ml, 5 ml, 10 min,,,, 0.45 μm, 3 结果与讨论 3.1 色谱行为, mol/l, 5 min,, 1 2,,,, 线性实验 1, r ,, mg/ml~0.04 mg/ml 3.3 定量限和检出限 (detection limit, DL) (quantitation limit, QL) (S/N) DL S/N=3, QL S/N=10

3 5, : 1915 Fig. 1 1 Chondroitin sulfate standard of chromatogram map Fig. 2 2 The chromatogram map of the sample Fig. 3 3 The chromatogram map of the blank reagent Fig. 4 4 The chromatogram map of the excipients

4 表 1 线性实验结果 Table 1 Linear experimental results C(mg/mL) (A) STD STD STD STD STD Y=60311X (r 2 ) 定量限 mg/ml 1~100 ml,, μg/ml, 10, S/N=10 : QL μg/ml*50 ml/0.1 g=1.164 mg/g 检出限 S/N=3, DL QL/10*3= 1.164/10*3 mg/g= mg/g 3.4 稳定性实验 h, RSD=0.62%, 24 h 3.5 精密度实验 6, 2.3.2,, RSD(%) g/100 g, (RSD) 0.1%,, 加标回收率实验 0.1 g 9, 50 ml, 3, 3, ( mg/ml) 6.0 ml 7.5 ml 9.0 ml,, 10 min,, 0.45 μm,,, 3 Table 2 表 2 精密度实验结果 The precision of experimental results (g) (mg/ml) (g/100g) (g/100g) RSD(%) % Table 3 表 3 加标回收率实验结果 Standard addition recovery experiment results (g) (mg/ml) (mg) (mg) (%) (%) RSD(%)

5 5, : ,, 98.5%~100.0%, 99.39%, (RSD) 0.6% 4 小结 [5] - - [12],, Anion HC, -,, Plaas ABC Acll, 2- ; 0~500 nmol/l AS4A,,,,,,,,,, ABC ACII, mmol/l 3 mmol/l,, -, ABC,, 3,,,,,,,,,,,,,,,, ;,, -,,,,,,, [13,14,15],,,,, mol/l,,,, [15],,,,,, 参考文献 [1],. [J]., 2010, 8(3): Cao YH, Peng GQ. Chondroitin sulfate in application of chondroitin sulfate in medicine [J]. Central South Pharmacy, 2010, 8(3): [2],. [J]., 2000, 5: Gao H, Liu K. Study on the determination of chondroitin sulfate by benzene three phenol Spectrophotometry [J]. Chin J Biochem Pharm, 2000, 5: [3],. [J]., 2009, 11(3): Jiang YH, Zang Y. Official methods for determination of chondroitin sulfate [J]. Food Drug, 2009, 11(3): [4],. [J]., 1998, 3: Mao L, Lv ZH. Determination of chondroitin sulfate in shark cartilage by indirect atomic absorption spectrometry [J]. Chin J Prev Med, 1998, 3: [5]. [J]., 1998, 5: Mao L. Determination of chondroitin sulfate by Ion Chromatography [J]. J China Med Univ, 1998, 5: [6],. [J]. :, 2000, 23(4): Xia CJ, Meng Q. Determination of chondroitin sulfate by Reversed Phase High Performance Liquid Chromatography [J]. J Anhwei Normal Univ (Nat Sci Edit), 2000, 23(4): [7],,,.

6 [J]., 2002, 11(4): 7 8. Niu ZY, Zhang XT, Liu G, et al. Determination of chondroitin sulfate by ion pair reversed phase high performance liquid chromatography [J]. Chem Anal Meterage, 2002, 11(4): 7 8. [8],,,. [J], 2002, 5: Bao LJ, Yang JC, He ZH, et al. Chondroitin sulfate in shark's fin enzymatic hydrolysis by high performance liquid chromatography [J]. J Instrum Anal, 2002, 5: [9],. HPLC [J]., 2002, 21(2): Shi RP, Zhou QY. HPLC for determination of chondroitin sulfate [J]. Shangdong Pharm Ind, 2002, 21(2): [10],. RP HPLC [J]., 2007, 38(9): Pang ZG, Tao LP. Determination of chondroitin sulfate by RP-HPLC [J]. J Chin Med Ind, 2007, 38(9): [11] GB/T [S]. GB/T determination of chondroitin sulfate [S]. [12],. HPLC ELSD [J]., 2006, 23(5): Lin YF, Sun JY. HPLC ELSD for Determine the content of compound film glucosamine chondroitin sulfate [J]. Chin J Mod Appl Pharm, 2006, 23(5): [13] David JI, Roman M. Determination of chondroitin sulfate content in raw materials and dietary supplements by high performance liquid chromatography with ultraviolet detection after renzymatic hydrolysis: single laboratory validation [J]. J AOAC Int, 2007, 90(3): 659. [14],. [J]., 2011, 32(2) : Yu HZ, Fan WH. Chondroitin sulfate content determination method is reviewed [J]. Chin J Biochem Drugs, 2011, 32(2) : [15],,,. [J]., 2013, 17(12): Xing HY, Zhao R, Shen CY, et al. Determination of glucosamine hydrochloride in compound chondroitin sulfate chondroitin sulfate tablets by high performance liquid chromatography [J]. Anhui Med, 2013, 17(12): 作者简介 ( 责任编辑 : 白洪健 ) 陈彩云, 主要研究方向为保健食品的质量检测 @qq.com

Microsoft Word - 3098-3102 20150611007-蔡伟江-二校

Microsoft Word - 3098-3102 20150611007-蔡伟江-二校 6 8 Vol. 6 No. 8 2015 8 Journal of Food Safety and Quality Aug., 2015 蔡伟江 *, 邓鹏飞, 刘光兰, 李丹 (, 519040) 摘要 : 目的, 方法 (4.6 mm 250 mm, 5.0 μm) ; : : : =70: 16: 14(V:V:V),, : 1.0 ml/min; : 40 ; : 10