山紫菀藥材的質(zhì)量標(biāo)準(zhǔn)研究
發(fā)布時(shí)間:2019-08-30 來(lái)源: 日記大全 點(diǎn)擊:
中圖分類號(hào) R28 文獻(xiàn)標(biāo)志碼 A 文章編號(hào) 1001-0408(2018)08-1057-04
DOI 10.6039/j.issn.1001-0408.2018.08.11
摘 要 目的: 建立山紫菀藥材的質(zhì)量標(biāo)準(zhǔn)。方法: 采用薄層色譜法(TLC)對(duì)藥材樣品進(jìn)行定性鑒別;測(cè)定藥材樣品水分、灰分、浸出物的含量;采用高效液相色譜法測(cè)定藥材樣品中阿魏酸的含量,色譜柱為Waters SunFire C18, 流動(dòng)相為乙腈-0.1%磷酸溶液(13 ∶ 87,V/V),流速為1.0 mL/min,檢測(cè)波長(zhǎng)為319 nm,柱溫為30 ℃,進(jìn)樣量為10 ?L。結(jié)果:山紫菀的TLC圖斑點(diǎn)清晰,分離度好,陰性對(duì)照無(wú)干擾。藥材樣品水分為7.6%~9.4%,總灰分為11.7%~19.6%,酸不溶性灰分為5.9%~14.1%,浸出物為25.4%~37.5%。阿魏酸檢測(cè)進(jìn)樣量線性范圍為0.021 2~0.636 8 ?g(r=0.999 9);定量限為2.25 ng,檢測(cè)限為0.75 ng;中間精密度、重復(fù)性、穩(wěn)定性試驗(yàn)的RSD均小于3.0%;加樣回收率為97.81%~100.59%(RSD=1.02%,n=9)。結(jié)論:初步擬定山紫菀藥材水分不得過(guò)10.0%,總灰分不得過(guò)19.0%,酸不溶性成分不得過(guò)12.0%,浸出物不得少于25.0%,阿魏酸含量不得少于0.1%;所建標(biāo)準(zhǔn)可為山紫菀藥材的質(zhì)量控制提供參考。
關(guān)鍵詞 山紫菀;質(zhì)量標(biāo)準(zhǔn);阿魏酸; 水分;灰分;浸出物;薄層色譜法;高效液相色譜法
ABSTRACT OBJECTIVE: To establish the quality standard of Ligularia fischeri. METHODS: TLC was used for qualitative identification of samples. The contents of moisture, ash and extract were determined. The content of ferulic acid in samples was determined by HPLC. The determination was performed on Waters SunFire C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid (13 ∶ 87,V/V) at the flow rate of 1.0 mL/min. The detection wavelength was set at 319 nm, and column temperature was 30 ℃. The sample size was 10 ?L. RESULTS: TLC spots were clear and well-separated without interference from genitive control. The moisture, total ash, acid-insoluble ash and extract of samples were 7.6%-9.4%, 11.7%-19.6%, 5.9%-14.1% and 25.4%-37.5%, respectively. The linear range of ferulic acid were 0.021 2-0.636 8 ?g(r=0.999 9). limited of quantation was 2.25 ng, the limited of detection was 0.75 ng. RSDs of intermediate precision, reproducibility and stability tests were all lower than 3.0%. The recoveries ranged 97.81%-100.59%(RSD=1.02%,n=9). CONCLUSIONS: The moisture, total ash and acid-insoluble ash of samples are no more than 10.0%, 19.0%, 12.0%; the extract and the content of ferulic acid are no less than 25.0% and 0.1%. Established standard can provide reference for quality control of L. fischeri.
KEYWORDS Ligularia fischeri; Quality standard; Ferulic acid; Moisture; Ash; Extract; TLC; HPLC
山紫菀為地方習(xí)用藥材,始載于宋代蘇頌所著的《圖經(jīng)本草》,具有“溫肺下氣,消痰止嗽”的功效,可用于風(fēng)寒咳嗽氣喘、虛勞咳吐膿血的治療,現(xiàn)代藥理研究表明,其具有抗炎作用[1]。山紫菀主要分布于我國(guó)四川省、湖北省、貴州省和東北地區(qū)等,其基源也不統(tǒng)一。東北地區(qū)習(xí)用的山紫菀來(lái)源為菊科植物蹄葉橐吾[Ligularia fischeri (Ledeb.) Turcz.]的干燥根及根莖,多生于林下或林緣陰濕草地[2]。吉林省內(nèi)蹄葉橐吾分布廣泛,資源豐富,延邊地區(qū)民眾常將其嫩葉“馬蹄葉”作為山野菜食用。但1997年版《吉林省藥品標(biāo)準(zhǔn)》及2009年版《遼寧省中藥材標(biāo)準(zhǔn)》(第一冊(cè))中收載“山紫菀”檢驗(yàn)項(xiàng)目較少,且沒(méi)有含量測(cè)定項(xiàng),無(wú)法有效地控制山紫菀藥材的質(zhì)量。已有報(bào)道多集中于研究山紫菀藥材的性狀特征和顯微鑒別[3-4],而對(duì)其薄層色譜鑒別、水分、灰分、浸出物和含量測(cè)定等項(xiàng)未作研究。筆者采集10批山紫菀藥材,對(duì)其薄層色譜、水分、總灰分、酸不溶性灰分、浸出物、含量測(cè)定等項(xiàng)目進(jìn)行了系統(tǒng)研究,制定了以山紫菀對(duì)照藥材為對(duì)照的薄層色譜鑒別和以阿魏酸為對(duì)照品的含量測(cè)定方法,旨在為山紫菀藥材質(zhì)量控制和評(píng)價(jià)標(biāo)準(zhǔn)的建立提供參考。
相關(guān)熱詞搜索:紫菀 藥材 質(zhì)量標(biāo)準(zhǔn) 研究
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