离子液体-超声辅助-固相萃取法提取富集急性子药材中的4种凤仙萜四醇皂苷
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摘要
建立了一种绿色、快速、高效萃取和富集中药急性子中4种凤仙萜四醇皂苷的方法。采用离子液体并结合超声辅助萃取急性子中的化学成分,利用固相萃取小柱富集提取液中的凤仙萜四醇皂苷。通过考察离子液体种类及用量、p H值、超声时间、固相萃取剂和洗脱剂等实验条件对提取率的影响,确立了最优萃取剂为[C6mim]Br,最优萃取条件:萃取剂用量为0.9 m L,提取液p H=7.0,超声为30 min,最优富集条件:固相萃取小柱填料为0.9 g CHP20/P120,上样流速为1.5 m L/min,洗脱剂为1.5 m L甲醇。在最优条件下,4种凤仙萜四醇苷加标回收率在92.1%~108.2%之间,相关系数范围为0.9945~0.9975,检出限范围为1.8~4.5μg/m L,RSD<3.9%。本方法与传统回流提取方法提取效果接近,可准确测定急性子中4种凤仙萜四醇苷含量。
A green,rapid and efficient method was developed for the extraction of 4 kinds of hosenkosides from the seeds of Impatiens balsamina L. The hosenkosides were extracted by ionic liquid,and then enriched by solid phase extraction. The effects of the kinds and volume of ionic liquid,p H value,ultrasonic time,solid phase extractant and eluent on the extraction fields were investigated and optimized. Under the optimum conditions,the recoveries of 4 kinds of hosenkosides were between 92. 1% and 108. 2%,the correlation coefficients were 0.9945-0.9975,and the detection limits were 1.8-4.5 μg/m L. The RSD values were all less than 3.9%. The experimental results showed that this method was fast,efficient,environmental protection.This study provided a reference for the extraction and enrichment of trace components in Chinese medicinal herbs.
A green,rapid and efficient method was developed for the extraction of 4 kinds of hosenkosides from the seeds of Impatiens balsamina L. The hosenkosides were extracted by ionic liquid,and then enriched by solid phase extraction. The effects of the kinds and volume of ionic liquid,p H value,ultrasonic time,solid phase extractant and eluent on the extraction fields were investigated and optimized. Under the optimum conditions,the recoveries of 4 kinds of hosenkosides were between 92. 1% and 108. 2%,the correlation coefficients were 0.9945-0.9975,and the detection limits were 1.8-4.5 μg/m L. The RSD values were all less than 3.9%. The experimental results showed that this method was fast,efficient,environmental protection.This study provided a reference for the extraction and enrichment of trace components in Chinese medicinal herbs.
引文
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2 ZHAO Liang-Qian.Jiangsu J.Tradit.Chin.Med.,2002,23(9):25赵良倩.江苏中医药,2002,23(9):25
3 MA You-Yun.Shanghai J.Tradit.Chin.Med.,2007,41(1):78马有运.上海中医药杂志,2007,41(1):78
4 Fu Y,Gao W,Yu J J,Chen J,Li H J,Li P.J.Pharmaceut.Biomed.,2012,64-65(4):64-71
5 WANG Wei,JU Cheng-Guo,ZHU Xu,ZHAO Huan-Jun.Chin.Tradit.Pat.Med.,2011,33(2):199-202王巍,鞠成国,朱旭,赵焕君.中成药,2011,33(2):199-202
6 Wang Y C,Lin Y H.Fitoterapia.2012,83(8):1336-1344
7 CHEN Ming-Xia,WANG Xiang-Li,ZHANG Yu-Jie.Chin.J.Chin.Mater.Med.,2006,31(11):928-929陈明霞,王相立,张玉杰.中国中药杂志,2006,31(11):928-929
8 TONG Miao-Miao,ZHAI Yan-Jun,WANG Tian-Min,LI Na.Chin.Tradit.Pat.Med.2011,33(7):1171-1174佟苗苗,翟延君,王添敏,李娜.中成药,2011,33(7):1171-1174
9 Chinese Pharmacopoeia Commission,Chinese Pharmacopoeia,vol.I,Beijing:The Medicine Science and Technology,2015:263中华人民共和国药典(一部).国家药典委员会.北京:中国医药科技出版社,2015:263
10 Wu Q,Jin Y R,Yao H,Liu Y,Li P,Li X W.Chem.Res.Chinese U.,2017,(5):1-5
11 LI Hui-Jun,YU Jun-Jie,LI Ping.China Patent,201010126336.4,2012李会军,于俊杰,李萍.中国专利,201010126336.4,2012
12 TAN Li-Na,LU Juan,ZHU Na,MENG Lei,ZHU Hong-Wei,LIU Yu-Wei,JIN Yong-Ri,LI Xu-Wen.Chin.J.Pharm.Anal.,2009,29(5):717-720谭丽娜,陆娟,朱娜,孟磊,朱红微,刘玉玮,金永日,李绪文.药物分析杂志,2009,29(5):717-720
13 Li H J,Yu J J,Li P.J.Pharmaceut.Biomed.,2011,54(4):674-680
14 Sara L,Héctor R,Alberto A,Ana S.Fluid Phase Equilibr.,2014,361(2):37-44
15 Xu W,Chu K D,Li H,Zhang Y Q,Zheng H Y,Chen R L,Chen L D.Molecules,2012,17(12):14323-14335
16 Ana F MCláudio,Ana M F,Mara G F,Jo2o A P C.Green Chem.,2013,15(7):2002-2010
17 Choi S A,Lee J S,Oh Y K,Jeong M J,Kim S W,Park J Y.Algal Res.,2014,3(1):44-48
18 YU Xiu-Pei,FENG Fang,TENG Bao-Qi,CHEN Yu-Yu.Pharm.Clin.Res.,2012,20(3):264-266于秀培,冯芳,滕宝褀,陈玉宇.药学与临床研究,2012,20(3):264-266
19 Xu J J,Li Q,Cao J,Warner E,An M R,Tan Z J,Wang S L,Peng L Q,Liu X G.J.Chromatogr.A,2016,1463(9):32-41
20 Yan H Y,Sun N,Han Y H,Yang C,Wang M Y,Wu R J.J.Chromatogr.A,2013,1307(17):21-26
21 Visser A E,Swatloski R P,Reichert W M,Griffin S T,Rogers R D.Ind.Eng.Chem.Res.,2000,39(10):3596-3604
22 Wang X Z,Li X W,Li L J,Li M,Wu Q,Liu Y,Yang J,Jin Y R.Anal.Methods,2016,8(35):6566-6572
23 Yang C,Sun Y Y,Kyung H R,Yan H Y.J.Chromatogr.A,2014,1361(26):53
24 CHEN Yi-Xin,FENG Qing-Sheng,WANG Xiao-Zhong,LI Lan-Jie,LI Xu-Wen,JIN Yong-Ri.Chinese J.Anal.Chem.,2016,44(7):1106-1111陈一鑫,冯清胜,王晓中,李兰杰,李绪文,金永日.分析化学,2016,44(7):1106-1111
25 Li H J,Liu Y,Yi Y T,Miao Q,Liu S J,Zhao F,Cong W,Wang C H,Xia C H.J.Chromatogr.B,2017,1048:56-63