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

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1 6 8 Vol. 6 No Journal of Food Safety and Quality Aug., 2015 L- * 叶少文 (, ) 摘要 : 目的, L-, L- 方法,,, Na, L- 结果 L ~ mg/ml, r> % 100% 120%, L- 97.2% 结论, L- 关键词 : ; ; L- Determination of free L-cysteine by automatic amino acid analyzer YE Shao-Wen * (By-Health Co., Ltd., Zhuhai , China) ABSTRACT: Objective By comparison of the traditional detection method for sulfur-containing amino acids, formic acid oxidation method, this paper puts forward a more simple operation method with accurate calculation of free L-cysteine content for those health food adding L-cysteine. Methods The sample was dissolved with buffer ultrasonic, filtered by microporous membrane filter, and analyzed by automatic amino acid analyzer. Na type ion exchange chromatography column separation was used. The content was calculated by L-cysteine standard quantitative calculation. Results The concentration of L-cysteine in the range of ~ mg/ml had a good linearity with peak area, the correlation coefficient r was > At the level of adding 80%, 100%, and 120%, the average recovery of L-cysteine was 97.2%. Conclusion The method is simple, accurate, reproducible and applicable for the determination of L-cysteine in health food. KEY WORDS: sulfur-containing amino acid; automatic amino acid analyzer; L-cysteine 1 引言 -SH, -SH, L- [1] GB/T , GB/T [2],,,, ( ), [3] L-,, L- [4], L-, GB/T [5],,, L-, L- * 通讯作者 :,, @qq.com *Corresponding author: YE Shao-Wen, Herbalists, By-Health Co., Ltd., Zhuhai , China @qq.com

2 [6] 2 材料与方法 2.1 试剂与仪器 L- (: 99.0%, :, : JS0925RC14) [7] ; [ (, )19.6 g+ (, )17.3 ml+(, )20 ml+(, )1.2 ml 1 L ]; 1[(, )19.6 g+ (, )13.5 ml+ (, )2 ml+(, )1.2 ml+ (, )20 ml 1 L ]; 2[ (, )19.6 g+ (, )9.3 ml+(, )1.2 ml 1 L ]; 3[(, )19.6 g+ (, )0.7 ml+ (, )58.4 g+(, )1.2 ml 1 L ]; 4[ (, )16 g 1 L ]; (biochrom, : ) [8] ; L- (: biochrom 30+) : biochrom Na+ Sodium Column 2.2 分析测试条件 : 20μL : ( ) (min) (ml/h) ON OFF Nin Rec commands ON OFF Reset ON OFF Load ON OFF ON OFF Reset ON ON ON ON ON ON ON ON ON ON ON ON OFF OFF OFF OFF OFF ON OFF : Nin, Rec : ( ) (min) (ml/h) Nin Rec ON ON ON ON ON ON OFF OFF OFF OFF OFF ON OFF 2.3 标准品溶液的配制 L mg 25 ml,, ml 10 ml, L mg/ml [9] 2.4 供试品溶液的配制 30 mg 25 ml, (40 khz)10 min [10],, 0.45 μm, [11] 2.5 线性实验 L-, 0.45 μm,,, (X), (Y),, [12] 2.6 重复性实验 6, 2.4,, RSD(%) [13] 2.7 加标回收实验 15 mg 9, 25 ml, 3, 3, L mg, 2.4, 0.45 μm, [14] 3 结果与分析 3.1 标准曲线确证结果 L- 1,

3 8 : L , L ~ mg/ml Table 1 表 1 标准曲线方程 The standard curve equation (r) L- Y=4919.5X 检出限和定量限 LOD LOQ (S/N) LOD S/N=3, LOQ S/N= 检出限 L- LOD=4.82 μg/ml, S/N=3, L- : 4.82 μg/ml 25 ml/1000/30 mg 100=0.004% 定量限 S/N=10 : LOQ LOD/3 10,, L- : 0.004/ % 3.3 重复性实验 L- 2, h, 2, (RSD) 1.3%, 12 h, 3.4 回收率实验 L- 3 3, 3 L- : 97.2%(RSD) 1.3% 3.5 实际样品的测定 2.2, L-( 1), L- L-, 2,, 表 2 重复性的实验 (n=6) Table 2 The precision of the experiment (n= 6) h (%) (%) RSD(%) L Table 3 表 3 加标回收率实验 (n=9) The standard addition recovery of experiment (n=9) (mg) (mg) (%) (%) RSD(%) L

4 L- Fig. 1 Chromatogram of L-cysteine standard 2 Fig. 2 Chromatogram of sample 4 讨论 GB/T ,,,,,, L-,,,,, 12 h, [15] L-,,, L- 参考文献 [1]. [J] (05): Sun MS. Amino acid analyzer using economic rationality research [J]. J Agric Technol, 2011, (5): [2],,,. [J]., 2001, (12):

8 : L- 3133 Sun W, Pan F, Zhang ZZ, et al. Collagen specific amino acid determination method to improve [J]. J Third Military Med Univ, 2001, (12): 20 22. [3],. [J]., 2005, (3): 62 64. Yu H, Mou SF.

5 8 : L Sun W, Pan F, Zhang ZZ, et al. Collagen specific amino acid determination method to improve [J]. J Third Military Med Univ, 2001, (12): [3],. [J]., 2005, (3): Yu H, Mou SF. The research progress of amino acid analysis method [J]. J Anal Chem, 2005, (3): [4],,. [J]., 2012, (5): Xing J, Li QL, Geng TH. The research progress of amino acid analysis method [J]. Chin Food Addit, 2012, (5): [5],,. [J]., 2012, (6): Cai M, Ji WL, Liu HL. Automatic amino acid analyzer method of rapid determination of hydroxyproline (hyp) in milk research [J]. Chin J Food Hyg, 2012, (6): [6],,. [J]., 2012, (34): Chen ZL, He XL, Zhang ZQ. Northern shaanxi jujube amino acid analysis [J]. Chin Agric, 2012, (34): [7],,. [J]., 2001, (2): Xiao LY, Liu N, Wang HF. Before a new column derivative method for the determination of plasma homocysteine [J]. J China-Japan Friendship Hospital, 2001, (2): [8],. [J]. ( ), 1999, (6): Hu HY, Liu JG. Blood homocysteine determination method and clinical significance [J]. Foreign Med Clin Biochem Inspection, 1999, (6): [9],,. [J]., 2008, (5): Cui XY, Cao MF, Sun H. Homocysteine metabolism and its clinical application [J]. Test Clin Med, 2008, (5): [10]. [J]., 2002, (4): Wang HL. Homocysteine detection and its application [J]. J Theory Pract Diagn, 2002, (4): [11],. - (Ⅲ)[J]., 2006, (3): Feng SL, Wang HQ. Adjacent dinitrogen fe - iron ( ) determination of cysteine [J]. J Xinyang Agric Coll, 2006, (3): [12],,. L- [J]., 2006, (Z1): Xi YQ, Yang M, Qiu HO. Dynamic fluorescence spectrophotometry [J]. J Spectrum Instrum Anal, 2006, (Z1): [13],,. [J]., 2005, (4): Liu WH, Zhang D, Li ZG. Indirect atomic absorption spectrometry determination of cysteine [J]. J Zhejiang Univ Technol, 2005 (4): [14],,. [J]. ( ), 2004, (2): Lan JG, Luo DB, Li MM. Phosphorus molybdenum heteropoly acid spectrophotometry cysteine [J]. J South-central Univ Nationalities (Nat Sci Ed), 2004, (2): [15] Li FM, Gai XM. System analysis of cysteine protease inhibitors (English) [J]. J Agric Sci Technol, 2010, (02): 作者简介 ( 责任编辑 : 白洪健 ) 叶少文, 西药师, 主要研究方向为保健食品的质量检测 @qq.com

Microsoft Word 王德伟-二校 3088

Microsoft Word 王德伟-二校 3088 6 8 Vol. 6 No. 8 2015 8 Journal of Food Safety and Quality Aug., 2015 王德伟 *, 游景水, 黄远英 (, 519040) 摘要 : 目的 (RP-HPLC) 方法 (ph 4.6), RP-HPLC, ph4.6, C 18, A 0.1%, B 0.09%(V:V) 90%(V:V),, 214 nm, 0.7 ml/min