6 4 Vol. 6 No. 4 2015 4 Journal of Food Safety and Quality Apr., 2015 赵 岩 1, 妙志岩 1, 牛淑静 2, 郜玉钢 1*, 蔡恩博 1, 杨鹤 1, 刘双利 1, 张连学 1* (1., 130118; 2., 130062) 摘要 : 目的 A 方法 (thin layer chromatography, TLC) ; (high performance liquid chromatography, HPLC) A 结果,, ; 0.5~50 µg, 98.53%~102.53%, (RSD) 0.84%~1.83% ; A 0.0006~0.06 mg/ml(r 2 =0.9998), 98.80%, RSD 0.89% 结论 A 关键词 : ; ; ; Study on quality control for Renshen Rongzhi capsules ZHAO Yan 1, MIAO Zhi-Yan 1, NIU Shu-Jing 2, GAO Yu-Gang 1*, CAI En-Bo 1, YANG He 1, LIU Shuang-Li 1, ZHANG Lian-Xue 1* (1. College of Chinese Medicine Material, Jilin Agriculture University, Changchun 130118, China; 2. Jilin Food & Drug Estimate Center, Changchun 130062, China) ABSTRACT: Objective To establish the methods to qualitatively identify the ginseng and Ganoderma lucidum spore powder, and determine the ginsenosides and ganoderic acid A in the Renshen Rongzhi capsules. Methods Qualitative identification of ginseng and ganoderma spore in Renshen Rongzhi capsules was carried out by thin layer chromatography (TLC). Ginsenosides and Ganoderma acid A were determined by high performance liquid chromatography (HPLC). Results The TLC spots were clear with high resolution, and the blank test showed no interference. The linear range of ginsenosides was 0.5~50 µg, the average recovery was between 98.53%~102.53%, and the relative standard deviation (RSD) was between 0.84%~1.83%. The linear range of ganoderma acid A was 0.0006~0.06 mg/ml (r 2 =0.9998), the average recovery was 98.80%, and the RSD was 0.89%. Conclusion The qualitative and quantitative analysis methods are applicable for the quality control of Renshen Rongzhi capsules. 基金项目 : (2011BAI03B01)(201303111) (2009GJB10031) (20130303094, 20140204013YY, YYZX201258, 20140311050YY) Fund: Supported by the National Science and Technology Support Program (2011BAI03B01), the National Nonprofit Industry Research and Special (201303111), the Ministry of Science and Technology Personnel Services Business Project (2009GJB10031) and the Jilin Province Science and Technology Development Programme (20130303094, 20140204013YY, YYZX201258, 20140311050YY) * 通讯作者 :,,, E-mail: gaoyugang_2006@163.com,,, E-mail: zlx863@163.com *Corresponding author: GAO Yu-Gang, Professor, Chinese Medicine Material College of Jilin Agricultural University, No.2888, Xincheng Street, Nanguan District, Changchun 130118, China. E-mial: gaoyugang_2006@163.com ZHANG Lian-Xue, Professor, Chinese Medicine Material College of Jilin Agricultural University, No.2888, Xincheng Street, Nanguan District, Changchun 130118, China. E-mial: zlx863@163.com
1370 6 KEY WORDS: Renshen Rongzhi capsules; thin layer chromatography; high performance liquid chromatography; quality control 1 引言 (Renshen Rongzhi capsules),, [1-6], [7-9], [10-12], [13], (thin layer chromatography, TLC) ; (high performance liquid chromatography, HPLC) A,,, 2 材料与方法 2.1 仪器与试剂 LC 3000 ( ); C 18 (4.6 mm 250 mm, 5 μm)(); LA 114 ( ); KQ-250 B ( ); ( ); DHG-9246 A ( ); FW-200 (); DSY-2-4 ( ) (, -B&J); ( ); ; ( ); A ( ) 2.2 实验方法 [1] 2.2.1 人参的薄层鉴别 1.0 g, 40 ml, 1 h,,, 0.5 ml, 10 ml, 30 min,, 3,,,, 1 ml, 0.7 g 0.3 g, Re Rg 1, 1 ml 2 mg, ( 2010 Ⅵ B), 1~2 μl, G, -- - (15:40:22:10)10,,,, 10, 105 [14-17] 2.2.2 灵芝的薄层鉴别 2.0 g, 30 ml, 30 min,,, 1 ml, 0.1 g 1.9 g, ( 2010 Ⅵ B), 4 μl, G, (60~90 )-- (12:8:1),,,, 365 nm 2.2.3 人参单体皂苷的含量测定 (1) C 18 (4.6 mm 250 mm, 5 μm); (A) (B), : 0 min(19.5% A), 24 min(21.5% A), 26 min(21.5%a), 30 min(29% A), 52 min(31.5% A), 55 min(38% A), 65 min(38% A); 1.0 ml/min; 35 ; 203 nm; : 20 µl (2) : Rg1 Re Rf Rb1 Rg2 Rc Rb2 Rb3 Rd 5 mg,
4, : 1371 5 ml,, 0.45 μm : 0.5 g, 3 h,,, 100 ml, 25 ml,,, 30 min,,, 5 ml,, 0.45 μm : 0.4 g,, : 0.1 g,, (3) (µg), (4), 6, Rg1 Re Rf Rb1 Rg2 Rc Rb2 Rb3 Rd RSD, (5), 0 2 4 6 8 24 h, Rg1 Re Rf Rb1 Rg2 Rc Rb2 Rb3 Rd RSD, (6), 2.2.3(2) 6,,,, Rg1 Re Rf Rb1 Rg2 Rc Rb2 Rb3 Rd RSD, (7),, (8), 3 2.2.4 灵芝酸 A 的含量测定 (1) C 18 (4.6 mm 250 mm, 5 μm); (A) 0.1% (B), : 0 min(35% A), 18 min(35% A), 18.01 min(100%a), 30 min(100% A), 30.01 min(35%a), 40 min(35%a); 0.8 ml/min; 25 ; 254 nm; 20 µl (2) : A,, 1 ml 0.06 mg : 2.0 g,,, 150 ml, 1 h,,,, 10 ml,, 0.45 μm : 0.1 g,,, : 1.9 g,,, (3) A 0.01 0.1 0.2 0.5 0.7 1.0 ml, 1 ml, 20 µl,,, (Y), (X), (4) A, 6,, RSD, (5), 0 2 4 6 8 24 h, RSD, (6), 2.2.4(2) 6,,, A, RSD, (7),, (8), 3 A
1372 6 3 结果与分析 3.1 人参的薄层鉴别,, 1 :,,,,, 2 :,,,, 1.2.3 ; 4. ; 5. 2 TLC Fig. 2 The chromatogram of Ganoderma 1.2.3 ; 4. ; 5. ; 6. 1 TLC Fig. 1 The chromatogram of Panax ginseng 3.2 灵芝的薄层鉴别, 3.3 人参单体皂苷的含量测定 3.3.1 色谱条件,, 3 9 Fig. 3 a. ; b. ; c. ; d. 3 HPLC The chromatogram of Renshen Rongzhi capsule and references
4, : 1373 3.3.2 线性关系考察 Rg1 Re Rf Rb1 Rg2 Rc Rb2 Rb3 Rd 0.5~50 µg, 9 1 表 1 9 种人参皂苷的标准曲线及样品含量 Table 1 The standard curve and the content of 9 kinds of ginsenosides r 2 (mg/g) (n=3) Rg1 Y=136537X+13036 0.9997 0.9469±0.0112 Re Y=342404X+12592 0.9996 0.2628±0.0032 Rf Y=292369X-5871.9 0.9997 0.2131±0.0021 Rb1 Y=180325X+1791.1 0.9995 0.2772±0.0023 Rg2 Y=174011X+6725.2 0.9997 0.0320±0.0003 Rc Y=97372X+12701 0.9994 0.3063±0.0038 Rb2 Y=283962X-12622 0.9997 0.1186±0.0016 Rb3 Y=243335X+2958.4 0.9994 0.0047±0.0001 Rd Y=248888X+174.82 0.9994 0.1744±0.0022 3.3.3 方法学考察, 2 2,, 24 h,, Table 2 表 2 方法学考察结果 The results of the studies on the method RSD(%) - 0.53%~0.89% - 0.78%~1.18% - 1.15%~1.64% 98.53%~102.53% 0.84%~1.83% 3.3.4 样品含量的测定 1 3.4 灵芝酸 A 的含量测定 3.4.1 色谱条件,, 4 A a. b. c. d. 1. A 4 HPLC Fig. 4 The chromatogram Renshen Rongzhi Capsule and References
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