research of Shencao Tongmai Keli effect on chronic heart failure rat cardiac function and BNP [J]. Liaoning J Tradit Chin Med( ), 2012, 39(4):706-708. [5] XUE F, HAO L, TANG B, et al. The research of Shenfu extract to sustain rat chronic heart failure model [J]. Pharmacol Clin Tradit Chin Med( ), 2007, 23(5): 41-43. [6] ZHANG Z W. The clinical effects of Shenqifuzheng injection in treating the chronic heart failure patients [J]. Contemp Med( ), 2011, 17(8): 1-2. [7] YANG Y C, CHENG H Y. Efficacy of benazepril combined with irbesartan in the treatment of chronic heart failure with proteinuria [J]. Chin J Mod Appl Pharm( ), 2012, 29(6): 560-563. [8] DU W X. Think about some issues of traditional Chinese medicine treatment of chronic heart failure//2011 Heart disease branch of China association of Chinese medicine annual meeting and Beijing Chinese medicine academic society of professional committee meeting on cardiovascular disease [C]. 2011: 215-218. [9] ZHANG Y, LIAO J D, WANG C L. The experimental research of the different compatibility of replenishing qi activating blood and promoting urination on the impact of chronic heart failure rats MMP-9 [J]. Lishizhen Med Mater Med Res( ), 2012, 23(8): 1937-1939. [10] YANG X G, LI B, The degree of heart failure classification and the severe heart failure diagnosis and treatment [J]. Chin Heart J( ), 2005, 17(1): 89-90. 2013-06-08 1 1,2 1* 1 1 1 1 1* (1. 130118 2. 132109) 6 ( )L- HPLC A GC-MS A L- 4 73 A L- (P<0.05) R284.1 B 1007-7693(2014)04-0416-06 DOI: 10.13748/j.cnki.issn1007-7693.2014.04.008 Comparative Research on Effective Components and Toxic Components of Asari Radix Et Rhizoma form Different Areas ZANG Pu 1, WU Xiaolin 1,2, GAO Yugang 1*, YANG He 1, ZHAO Yan 1, MA Ling 1, WANG Xiaohan 1, ZHANG Lianxue 1* (1.College of Traditional Chinese Medicine, Jilin Agricultural University, Changchun 130118, China; 2.Jilin Agricultural Science and Technology College, Jilin 132109, China) ABSTRACT: OBJECTIVE To study the difference of effective components and toxic components of Asari Radix et Rhizoma form different areas. METHODS Asari Radix et Rhizoma from six areas(fengcheng, Tonghua, Antu, Benxi, Dunhua and Harbin) were used as experimental materials. The contents of total aristolochic acid and L-tyrosine were detected by colorimetry method. HPLC was used to determine the contents of aristolochic acid A and asarinin. The types and contents of volatile oil were analyzed by GC-MS method. RESULTS The areas with highest content of total aristolochic acid, aristolochic acid A, L-tyrosine and asarinin were Benxi, Fengcheng, Harbin and Fengcheng, respectively. The areas with lowest contents of the 4 components were Harbin, Antu, Antu and Tonghua. Essential oils of asarum in different areas contained 73 kinds of compounds, and the content of safrole, methyleugenol, myristicin and elemi were higher. The content of safrole in Asari Radix et Rhizoma in (2011BAI03B010602) (2012ZX09304006) (20112101 20110228 20130102075JC) E-mail: zangpu@163.com * E-mail: gaoyugang_2006@163.com E-mail: zlxbooksea@163.com 416 Chin J Mod Appl Pharm, 2014 April, Vol.31 No.4 2014 4 31 4
the sequence of decending were Tonghua, Fengcheng, Benxi, Antu, Dunhua and Harbin; the content of methyleugenol in the sequence decending were Fengcheng, Tonghua, Benxi, Antu, Dunhua and Harbin; the content of myristicin in the sequence of decending was Dunhua, Antu, Fengcheng, Tonghua, Benxi and Harbin; the content of elemicin from high to low were as follows: Fengcheng, Tonghua, Antu, Benxi, Dunhua and Harbin. CONCLUSION The results reveal that the contents of total aristolochic acid, L-tyrosine, aristolochic acid A and asarinin were significantly different in different areas(p<0.05). KEY WORDS: Asari Radix et Rhizoma; quality evaluation; effective component; toxic ingredient Asarum heterotropoides Fr. Schmidt var. mandshuricum (Maxim.) Kitag. A. sidboldii Miq.var. seoulense Nakai. A. sidboldii Miq. [1] [2] [3-4] [5] [6] 63 2 176 1 2008 9 Asarum heterotropoides Fr. Schmidt var. mandshuricum (Maxim.)Kitag. 2008 9 A. sidboldii Miq.var.seoulense Nakai. 0.25 mm A ( SLBC9609V >98%) L- ( ZBB10220 >98%) ( International Laboratory) (Alfa Aesar) ( Fisher Scientific ) ( International Laboratory 1303251 >98%) ( Caledon Laboratories LTD.) ( TEDIA COMPANY, INC) 754 LC-2010A Agilent 6890N25973N GC2MSD / 2 2.1 A L- [7] A Shim-Pack C 18 (150 mm 4.6 mm 5 µm) -1% (72 28) 1.0 ml min 1 30 315 nm [8] - (50 50) 1.0 ml min 1 35 240 nm [9] - (99 1) 1.0 ml min 1 25 230 nm [10] 2.2 [11] GC-MS HP-5(0.25 mm 30 m 0.25 µm) 260 60 10 min 1 100 6 min 1 260 41.67 min 1.0 ml min 1 EI 70 ev 1 µl 200 3 3.1 A A (P<0.05) 1 A (P>0.05) 4 4 2014 4 31 4 Chin J Mod Appl Pharm, 2014 April, Vol.31 No.4 417
1 A Tab 1 The contents analysis of total aristolochic acid, aristolochic acid, asarinin and tyrosine of Asari Radix et Rhizoma from different areas /mg g 1 A /µg g 1 /mg g 1 L- /µg g 1 0.307 9±0.003 0 18.900 7±0.071 3 0.408 2±0.005 7 0.170 0±0.013 2 0.440 2±0.005 0 20.647 0±0.274 7 0.432 2±0.001 6 0.662 1±0.054 2 0.202 6±0.003 9 16.621 1±0.134 8 0.662 6±0.005 7 0.369 1±0.027 9 0.423 1±0.005 6 24.937 8±0.078 0 0.444 3±0.000 6 1.446 7±0.113 5 0.633 3±0.009 1 10.575 5±0.107 8 0.447 6±0.004 2 1.170 7±0.099 6 0.388 5±0.009 8 6.592 0±0.252 1 0.327 0±0.005 3 1.015 2±0.104 9 3.2-1 NIST 73 2 (33.407%) (30.768%) (27.258%) (24.518%) (20.832%) (14.879%) (8.065%) (8.032%) (5.738%) (4.978%) (3.931%) (3.922%) (13.026%) (11.960%) (11.873%) (9.135%) (7.409%) (5.807%) 1 Fig 1 The total ion chromatogram of Asari Radix et Rhizoma 2 GC-MS Tab 2 The GC/MS analysis of volatile oil in Asari Radix et Rhizoma /% 1 C 10 H 16 136 0.023 0.018 2 C 10 H 16 136 0.016 0.010 0.007 3 β- C 10 H 16 136 0.021 0.082 0.025 0.015 0.022 4 β- C 10 H 16 136 0.122 0.014 0.015 0.011 0.006 5 α- C 10 H 16 136 0.014 0.009 0.024 0.010 6 -α C 10 H 16 136 0.032 0.093 0.027 0.052 0.024 7 2- C 10 H 14 134 0.037 0.016 0.019 0.009 8 C 10 H 16 136 0.034 0.011 9 C 10 H 18 O 154 0.161 0.111 0.132 0.051 0.011 10 1- -4-(1- ) C 10 H 16 136 0.054 0.028 0.012 11 C 10 H 16 O 152 0.093 0.086 0.101 0.048 0.027 12 2,6,6-,2,4-1- C 10 H 14 O 150 0.751 1.332 0.523 0.880 0.172 0.153 13 C 10 H 18 O 154 1.222 0.724 0.989 0.808 0.709 0.485 14 4- -1-(1- )-3-1- C 10 H 18 O 154 0.254 0.191 0.200 0.189 0.115 0.120 15 C 10 H 14 O 150 0.133 0.138 0.145 0.079 0.114 0.224 16 C 10 H 12 O 148 0.171 0.409 0.163 0.157 0.044 0.068 17 2- -5- C 11 H 16 O 164 0.099 0.026 0.032 18 C 10 H 14 O 150 0.139 0.131 0.075 0.093 0.084 418 Chin J Mod Appl Pharm, 2014 April, Vol.31 No.4 2014 4 31 4
/% 2 19 1,3- -5- C 9 H 12 O 2 152 12.489 10.280 11.361 7.844 6.024 5.936 20 / C 10 H 10 O 2 162 13.026 11.873 11.960 9.135 7.409 5.807 21-2- C 15 H 14 O 2 226 0.060 0.084 0.075 0.101 0.094 22 4- -2- - C 9 H 10 O 2 152 0.140 0.151 0.140 23 2- -3-(2- ) C 10 H 12 O 2 162 0.211 0.109 0.387 0.193 0.084 24 C 11 H 14 O 2 178 30.768 27.258 33.407 24.518 20.832 14.879 25 C 10 H 14 O 3 182 8.023 4.978 8.065 5.738 3.931 3.922 26 3,9- C 12 H 18 162 0.270 0.143 0.268 0.097 0.410 0.412 27 C 11 H 12 O 3 190 11.257 10.934 12.547 14.249 17.049 8.369 28 C 15 H 22 202 0.198 0.161 0.234 0.179 0.270 0.210 29 β- C 15 H 24 204 0.148 0.190 0.260 0.307 0.238 30 C 15 H 32 212 2.836 3.066 1.461 3.745 2.441 2.886 31 3,4,5- C 10 H 12 O 5 222 0.138 0.147 0.170 0.226 0.322 0.067 32 3,4-( ) C 10 H 10 O 3 178 1.911 1.317 1.242 1.592 1.432 0.746 33 C 12 H 16 O 3 208 1.858 5.569 2.428 1.739 1.683 1.314 34 S-(Z)-3,7,11- -1,6,10- C 15 H 26 O 222 0.741 0.705 0.678 0.821 1.989 0.567-3- 35 C 15 H 24 O 220 0.395 0.295 0.341 0.367 0.443 0.267 36 C 15 H 26 O 222 0.198 0.376 0.444 0.314 0.436 0.365 37 3,3,5- -2-(3- )-2- C 16 H 26 O 234 0.180 0.229 0.189 0.157 0.268 38 2- -4,5-( ) C 10 H 10 O 4 194 3.883 3.768 3.798 4.978 3.925 2.965 39 C 15 H 26 O 222 0.457 0.677 0.582 0.358 0.400 0.407 40 C 10 H 12 O 4 194 0.341 0.309 0.325 0.517 0.487 0.315 41 2,4- -3- C 12 H 16 O 3 208 0.502 1.088 0.546 0.631 0.399 0.277 42 C 16 H 34 226 0.292 0.230 0.110 0.274 0.302 0.225 43 C 15 H 24 O 220 0.176 0.256 0.151 0.166 0.304 0.165 44 C 15 H 30 O 2 242 0.039 0.078 0.022 0.354 0.295 0.628 45 ( ) C 16 H 32 O 2 256 0.695 1.612 0.422 3.625 4.329 10.518 46 C 18 H 32 O 2 280 0.201 1.078 0.312 47 C 18 H 30 O 2 278 0.109 6.196 7.417 48 C 18 H 36 O 2 284 0.030 0.155 0.076 0.498 14.761 49 C 20 H 42 282 0.142 0.444 50 7- C 26 H 54 366 0.241 1.004 51 2- C 12 H 26 O 186 0.044 0.442 52 C 10 H 18 O 154 0.493 0.343 0.441 0.324 0.114 0.224 53 α- C 15 H 24 204 0.063 0.057 0.081 0.057 54 C 15 H 26 O 222 0.493 0.631 0.654 0.319 0.319 0.476 55 α- C 15 H 24 204 0.207 1.183 0.346 0.362 0.470 0.366 56 C 10 H 16 O 152 0.133 0.034 0.140 0.054 0.086 57 (S)-3-Methyl-6β-isopropenyl -2-cyclohexene-1-one C 10 H 14 O 150 0.087 0.115 0.035 0.068 5.936 58 C 20 H 38 278 0.113 0.112 0.135 0.273 0.150 59 z-8-methyl-9-tetradecenoic acid C 15 H 28 O 2 240 0.127 0.143 0.113 0.274 60 2(1H)Naphthalenone,3,5,6,7,8,8a -hexahydro-4,8a-dimethy l-6-(1-methylethenyl)- 61 4,6,6-Trimethyl-2-(3-methylbuta-1,3 -dienyl)-3-oxatricyclo[5.1.0.0(2,4)]octane C 15 H 22 O 218 0.049 0.120 0.118 0.098 0.135 0.080 C 15 H 22 O 218 0.139 0.181 0.246 0.284 0.397 0.221 62 9-Heptadecene-4,6-diyn-8-ol, (Z) C 17 H 26 O 246 0.165 0.245 0.204 0.269 0.273 0.129 63 naphthalene,decahydro-1,1-dimethyl- C 12 H 22 166 0.057 0.131 0.124 0.443 1.126 0.762 64 Kaura-16-ene C 20 H 32 272 0.083 0.084 0.116 0.118 0.191 2014 4 31 4 Chin J Mod Appl Pharm, 2014 April, Vol.31 No.4 419
/% 2 65 Cyclohexene,6-butyl-1-nitro- C 10 H 17 NO 2 183 0.039 0.050 0.131 0.118 0.221 66 N-Isobutyl-(2E,4Z,8Z,10E) -dodecatetraenamide 67 6-(1,1-Dimethylethyl)-dihydropyran-2,4-di one C 16 H 25 NO 247 0.126 0.266 0.189 1.874 1.507 2.396 C 9 H 14 O 3 170 0.007 68 Nonylcyclopropane C 12 H 24 168 0.148 0.242 0.192 0.174 0.230 69 nerolidol C 15 H 26 O 222 0.279 0.333 0.282 0.342 0.289 0.204 70 α-bulnesene C 15 H 24 204 0.239 1.005 0.584 0.658 0.733 0.636 71 (+)-δ-cadinene C 15 H 24 204 0.138 1.120 0.258 0.266 0.226 0.210 72 (1.α,4a.α,8a.α)-1,2,3,4,4a,5,6,8a-Octahydr o-7-methyl-4-methylene-1-(1-methylethyl) -naphthalene C 15 H 24 204 0.270 0.531 0.268 0.353 0.410 0.412 73 1-(3,4-Dimethoxy-phenyl)-propan-1-one C 11 H 14 O 3 194 0.285 0.210 0.269 0.268 0.218 0.176 97.868 97.974 98.658 98.007 84.796 98.038 4 73 A 3 3 6 REFERENCES [1] Ch.P(2010)Vol I( 2010. ) [S]. 2010: 214 [2] LIU J. According to the research on the volatile oil from different parts of Herba Asari to study its usage [J]. Res Tradit Chin Med( ), 1999(6): 54-55. [3] WANG B X. Modern Pharmacology and Clinic of Chinese Traditional Medicine( )[M]. Tianjin: Tianjin Science & Technology Translation Publishing, 2004: 982. [4] ZANG Y, SONG Z Y, WANG L L. Pharmacological effects and clinical application of Herba Asari [J]. China Pharm( ), 2007, 16(14): 62-63. [5] LIU J, MENG L, YUAN Z M, et al. Preliminary study on material basis of Asari Radix et Rhizoma against asthma and cough [J]. Her Med( ), 2012, 31(11): 1412-1415. [6] HUANG S W. TLC identification of aristolochic acid of Asarum heterotropoides Fr. [J]. Anhui Med Pharm J( ), 2003, 7(4): 299-300. [7] SHANG M Y, LI J, HU B. Determination of total aristolochic acid in the stem of Aristolochia manshuriensis [J]. Chin Tradit Herbal Drugs( ), 2000, 31(l2): 899-900. [8] GAO J, LI W, WEI F. Quantitative analysis of aristolocluc acid A in Asarum sieboldii by HPLC [J]. Chin Pharm J( 420 Chin J Mod Appl Pharm, 2014 April, Vol.31 No.4 2014 4 31 4
), 2005, 40(20): 1579-1580. [9] ZHANG L, CEN X H,,LIU Y L. RP-HPLC simultaneous determination of L-asarinin, L-sesamin and kakuol in Asarum heterotropoides Fr Schmidt var. mandshuricum(maxim.) Kitag [J]. Chin Tradit Herb Drugs( ), 2008, 39(7): 1098-1099. [10] HUANG X Z, JIANG W Z, HUANG M, et al. Determination of tyrosine from Stizolohium cochinchinensis(lour.) Tang et Wang [J]. China Pharm( ), 2009, 18(20): 23-24. [11] ZHANG Y Y, SONG X X, SUN H, et al. Analysis of the volatile oil of Herba Asari of Tonghua by GC-MS [J]. Spec Wild Economic Animal Plant Res( ), 2007(4): 56-66. 2013-04-11 1 2 (1. 365000 2. 365001) 2 HPLC R917.101 A 1007-7693(2014)04-0421-04 DOI: 10.13748/j.cnki.issn1007-7693.2014.04.009 Determination of Costuslactone in Muxiang Shunqi Pills By QAMS LAI Zengfa 1, XIA Lizhen 2 (1.Institule for Drug Control of Sanming Cify, Sanming 365000, China; 2.Sanming Cooperation of Chinese and Western Medicine Hospital, Sanming 365001, China) ABSTRACT: OBJECTIVE To establish a method for determinaion of two costuslactone in Muxiang Shunqi pills by quantitative analysis of multi-components by single marker(qams) for more perfect quality. METHODS Taking costunolide, as reference, a relative correction factor(rcf) of dehydrocostuslactone was established. Then the RCF was used to calculate the contents of the dehydrocostuslacton. In this way, the calculated value was compared with the external standard method. RESULTS No significant differences were found in the quantitative analysis results of dehydrocostuslacton between external standard method and QAMS method. CONCLUSION The described method is reliable, accurate, and can be used to control the quality of costuslactone of Muxiang Shunqi pills. KEY WORDS: Muxiang Shunqi pills; costuslactone; QAMS; HPLC 10 2 2010 [1] 1 Agilent 1200 ( Agilent ) LC-2010A ( ) Ultimate XB-C 18 (4.6 mm 250 mm 5 µm) Hyperclone C 18 (4.6 mm 250 mm 5 µm) Agilent Tc-C 18 (4.6 mm 250mm 5 µm) Waters sunfire C 18 (4.6 mm 250 mm 5 µm) BP211D ( ) KQ5200DE ( ) ( 111524-201107) ( 111525-201008) 100% Tel: (0598)8953906 E-mail: smgy_128@163.com 2014 4 31 4 Chin J Mod Appl Pharm, 2014 April, Vol.31 No.4 421