5 Tab. 5 Results of variance analysis F A 0.589 2 0.295 22.9 B 0.065 0 2 0.032 5 2.5 C 0.286 2 0.143 11.14 D( ) 0.025 8 2 0.012 9 F [4] F 0.05(2,2) =19 F 0.01(2,2) =99 Note: Chek the table of F values [4] F 0.05(2,2) =19, F 0.01(2,2) =99. Rb 1 D e F 4 5(A 2 B 2 C 3 D 1 ) Rb 1 A 2 B 1 C 3 D 1 Rb 1 A 2 B 2 C 3 D 1 12 h 15 60% 1.0 ml min 1 12 h 0.5 mol L 1 NaOH ph 7 60% 60% 3 L 9 (3 4 ) Rb 1 1.0 ml min 1 [5] D101 D201 D101+DA201(1 1) REFERENCES [1] CAI X, LIU Z G, WANG P X, et al. Study on purification process of ginsenoside with macro- reticular resin [J]. Chin Tradit Pat Med( ), 2001, 23(9): 631-634. [2] ZHANG C X, ZHENG Y L, ZHANG C H, et al. Study on extractive technology for total saponins and rebirth with macroreticular resin [J]. Chin Pharm J( ), 2003, 38(9): 661-664. [3] WU Q, CHEN X C, DU S Y. Study on enrichment of total ginsenosides from folium ginseng by technique of macroporous adsorptive resin [J]. J Beijing Univ Tradit Chin Med( ), 2006, 29(5): 344-346. [4] ZHANG C H, ZHOU Y Z, LIU Y F. Mathematical statistics method( ) [M]. Jinan: Shandong University Press, 1995. [5] ZHU H, HOU S X, SUN Y Y, et al. Macroporous resin adsorption and purification of effective components of different traditional Chinese medicine characteristics [J]. China J Chin Mater Med( ), 1998, 23(10): 607-609. 2013-09-09 * ( 350122) HPLC HPLC Lichrocart C 18 (250 mm 4.0 mm 5 µm) -0.1% ( ) 1.0 ml min 1 284 nm 30 8 80.55%~95.93%>95% >0.999 HPLC (2012J01386)(2010Y2004 2010J01189) ([2011]1598 ) Tel: 13960901707 E-mail: hqdhuang@163.com * Tel: (0591)22861135 E-mail: gscd2@163.com 1078 Chin J Mod Appl Pharm, 2014 September, Vol.31 No.9 2014 9 31 9
R943 B 1007-7693(2014)09-1078-05 DOI: 10.13748/j.cnki.issn1007-7693.2014.09.011 Investigation of Transfer Rates of Active Compounds in the Preparation Process of Daidai Flavonoids SMEDDS Soft Capsule HUANG Qingde, CHENG Qing, CHEN Dan *, ZENG Lingjun(Department of Pharmacy, Fujian University of Traditional Chinese Medicine, Fuzhou 350122, China) ABSTRACT: OBJECTIVE To study the transfer rates of active compounds in preparation process of Daidai flavonoids SMEDDS soft capsule upon HPLC characteristic fingerprint considering the property of multiple components in total flavonoids active part of Daidai. METHODS HPLC characteristic fingerprint was adopted with chromatographic column Lichrocart C 18 (250 mm 4.0 mm, 5 µm). Mobile phase was methanol-water with 0.1% phosphoric acid(gradient elution). The flow rate was 1.0 ml min 1 and the detection wavelength was set at 284 nm. The column temperature was controlled at 30. RESULTS The transfer rates of eight common peaks were between 80.55% and 95.93% in the preparation process of Daidai flavonoids SMEDDS soft capsule. The transfer rates of main characteristic compounds naringin and neohesperidin were >95%. And the similarity of holistic transfer rate of each active couponents was >0.999. CONCLUTION The preparation technology of Daidai flavonoids SMEDDS soft capsule can reserve the main active compouds in Daidai total flavonoids extract relative completively. KEY WORDS: the total flavonoids of Daidai; SMEDDS soft capsule; the transfer rate; HPLC characteristic fingerprint (Citrus Aurantium L. var daidai) >75% [1-4] [5-7] (self-microemulsifying drug delivery system SMEDDS) [8-9] HPLC 1 1.1 Waters 2695 ( Waters Waters 2996 Empower 3 ) XS 205 ( - ) TGL-18G-C ( ) KQ3200 ( ) 1.2 ( ) ( 20111102 20111104 20111106 20111110 20111112 20111114) ( 110722-200609 >98%) ( 111857-201001 >98%) 2 2.1 Lichrocart C 18 (250 mm 4.0 mm 5 µm) (A)-0.1% (B) 0~15 min 10%A 18%A 15~25 min 18%A 25~40 min 18%A 23%A 40~55 min 23%A 18%A 55~60 min 18%A 10%A 1.0 ml min 1 284 nm 30 10 µl 3 000 60 min 2.2 2.2.1 75% 2 2 h 1 6 2014 9 31 9 Chin J Mod Appl Pharm, 2014 September, Vol.31 No.9 1079
20.0 mg 25 ml 20 ml 5 min 5.0 ml 10 ml 2.2.2 ( ) 10.0 mg 25 ml 20 ml 5 min 5.0 ml 10 ml 2.2.3 100.0 mg 25 ml 20 ml 5 min 2.3 2.3.1 6 (relative retention time RRT) (peak area ratio PAR) RRT RSD 0.06%~0.13% PAR RSD 0.08%~2.76% RSD 0.06%~3.46% 2.3.2 6 2.2 2.1 RRT PAR 6 RRT RSD 0.07%~0.18% PAR RSD 0.07%~2.86% RSD 0.52%~3.85% 2.3.3 0 2 4 8 12 24 h RRT PAR RRT RSD <0.2% PAR RSD<2.3% RSD 0.35%~2.96% 24 h 2.4 10 µl 2.1 2.5 12 8 8 0.1 mg ml 1 [ =( / ) 100%] 1 2 1 Tab. 1 The translated common peaks of Chinese herbal medicines, intermediates, products during Daidai flavones SMEDDS soft capsule preparation 1 40 339 2 16 384 3 4 468 4 8 068 5 21 969 6 3 972 7 57 839 21 643 17 955 8 945 038 749 815 719 326 9 51 881 35 579 30 706 10 1 241 185 966 959 920 659 11 6 951 28 679 23 100 12 35 231 28 592 13 16 756 36 197 30 414 14 61 009 53 984 2 HPLC Tab. 2 The mobility value of the common peak area during Daidai flavones SMEDDS soft capsule preparation by HPLC /% 7 82.96 8 95.93 9 86.30 10 95.21 11 80.55 12 81.16 13 84.02 14 88.49 2.6 SPSS 6 1080 Chin J Mod Appl Pharm, 2014 September, Vol.31 No.9 2014 9 31 9
6 HPLC 8 Pearson Pearson 1.000( 0.01) 0.999~1.000 3 HPLC 1( ) 3 6 HPLC Tab. 3 The results of similar degree of the samples 6-1.000 0.999 1.000 1.000 1.000 0.999 1.000 3 HPLC HPLC HPLC HPLC 80.55%~ 95.93% >95% HPLC 8 Pearson 0.999 REFERENCES 1 HPLC A B C 8 10 Fig. 1 The HPLC chromatograms A raw Daidai; B the effective parts of daidai flavones; C Daidai flavones SMEDDS soft capsule; 8 naringin; 10 neohesperidin. [1] RAN X D. Zhong Hua Yiao Hai( ) [M]. Harbin: Haerbin Press, 1933: 964. [2] XIAO P G. Modern Chinese Material Medica() [M]. Beijing: Chemical Industry Press, 2002: 446. [3] LIU Y J, CHEN D, HUANG Q D, et al. Study on extraction techniques of favonoids in Citrus Aurantium [J]. Chin J Hosp 2014 9 31 9 Chin J Mod Appl Pharm, 2014 September, Vol.31 No.9 1081
Pharm( ), 2009, 29(21): 1826-1828. [4] CHEN D, LIU Y J. The preparation method of favonoids in Citrus aurantium, China, CN201010556341.9 [P]. 2011-05-18. [5] QIU H X, CHEN D, LIU Y J, et al. Study on antiatheroscloresis effects of Daidai Flavones Dropping pills on hyperlipidemia rats [J]. Chin J Mod Appl Pharm ( ), 2011, 28(7): 597-601. [6] LIU Y J, CHEN D, QIU H X, et al. In vitro antioxidant effect of the total flavones of Citrus aurantium L. var Daidai Tanaka fruits [J]. Chin J Mod Appl Pharm( ), 2012, 29(2): 97-101. [7] ZENG L G, CHEN D, ZHENG L, et al. Study on quality standard of daidai flavone extract [J]. Drug Standards China ( ), 2013, 14(5): 337-341. [8] LIU Y, ZHANG P, FENG N, et al. Optimization and situ intestinal absorption of self-microemulsifying drug delivery system of oridonin [J]. Int J Pharm, 2009, 365(1/2): 136-142. [9] GANG Y, YAN L. Preparation, characterization and evaluation of self-microemulsifying drug delivery systems (SMEDDSs) of Ligusticum chuanxiong oil [J]. Biomed Prev Nutr, 2010, 1(1): 36-42. 2013-12-13 1 1 1 1 2 1* (1. 323000 2. 325035) (brain derived neurotrophic factor BDNF) BDNF Zeta BDNF BDNF 30 600 r min 1 1 5 BDNF (178.7 22.1)nm Zeta 29.8 mv 4 (60±10)% 30 d BDNF BDNF 3 (P<0.05 P<0.01) BDNF BDNF R943 B 1007-7693(2014)09-1082-05 DOI: 10.13748/j.cnki.issn1007-7693.2014.09.012 Study on Preparation of Flexible Nano Liposome and Drug Delivery Efficiency of Brain XU Yanyan 1, YANG Junyan 1, HU Jieru 1, HE Weizhen 1, ZHAO Yingzheng 2, TIAN Weiqiang 1* (1.Department of Pharmacy, Lishui Central Hospital, Lishui 323000, China; 2.School of Pharmacy, Wenzhou Medical University, Wenzhou 325035, China) ABSTRACT: OBJECTIVE To prepare brain targeting brain derived neurotrophic factor-flexible nano liposome(bdnf-fnl), screening and optimization of preparation process using the brain derived neurotrophic factor (BDNF) as model drug, and to evaluate the quality of preparation. METHODS Intranasal brain targeting drug delivery system of BDNF-FNL were prepared by injection. The evaluation index were the morphology, particle size, entrapment efficiency and Zeta potential. The size distribution of BDNF-FNL were studied that related to influences of stirring temperature, stirring speed and the volume ratio of alcohol to water. And orthogonal design was adopted to obtain the optimal preparation technology based on the influences. Drug brain targeting delivery efficiency of flexible nano liposome was evlauted by determination of BDNF concentration in the brain. RESULTS The results of orthogonal test showed that the best preparation method was as follows: stirring temperature was 30, stirring speed was 600 r min 1 and the volume ratio of alcohol to water was 1 5. BDNF-FNL were round shape, particle size of (178.7±22.1) nm, and zeta potential of 29.8 mv. The preparation of stable storage for 30 d at 4, relative humidity (LQ12H30001) Tel: (0578)2681490 E-mail: xyy0412099@126.com (0578)2681483 E-mail: lstianwq@126.com * Tel: 1082 Chin J Mod Appl Pharm, 2014 September, Vol.31 No.9 2014 9 31 9