黃小蘭 何旭峰 周濃 陽文武 錢林群
中圖分類號 R284.1 文獻(xiàn)標(biāo)志碼 A 文章編號 1001-0408(2021)20-2473-06
DOI 10.6039/j.issn.1001-0408.2021.20.07
摘 要 目的:建立浙貝母配方顆粒的指紋圖譜,并測定其中3種成分的含量。方法:采用高效液相色譜(HPLC)法。以貝母素乙為參照,采用《中藥色譜指紋圖譜相似度評價系統(tǒng)(2012版)》繪制13批浙貝母配方顆粒的HPLC指紋圖譜,并進(jìn)行相似度評價,確定共有峰;采用相同的HPLC法測定浙貝母配方顆粒中貝母辛、貝母素甲和貝母素乙的含量,并比較不同生產(chǎn)企業(yè)樣品的質(zhì)量差異。結(jié)果:13批浙貝母配方顆粒中共有5個共有峰,相似度為0.669~0.971;指認(rèn)了貝母辛、貝母素甲和貝母素乙等3個共有峰。貝母辛、貝母素甲和貝母素乙檢測質(zhì)量濃度的線性范圍分別為30.00~180.00 μg/mL(r=0.999 9)、79.58~477.50 μg/mL(r=0.999 6)、97.33~584.00 μg/mL(r=0.999 4);精密度、穩(wěn)定性(24 h)、重復(fù)性試驗(yàn)的RSD均小于3%;平均加樣回收率分別為95.82%(RSD=1.17%,n=6)、99.00%(RSD=1.96%,n=6)、95.39%(RSD=2.00%,n=6)。13批樣品中,貝母辛、貝母素甲、貝母素乙的含量分別為0.17~1.02、0.52~2.26、0.70~3.50 mg/g,平均總含量為3.62 mg/g。其中,企業(yè)C、A樣品中上述成分的平均總含量較高,分別為5.02、4.61 mg/g,其次是企業(yè)E、B樣品,分別為3.48、3.02 mg/g;最低為企業(yè)D樣品,僅為1.87 mg/g。結(jié)論:所建指紋圖譜和含量測定方法簡便、可行,重復(fù)性好,可用于浙貝母配方顆粒的質(zhì)量評價;不同生產(chǎn)企業(yè)樣品的含量存在一定差異。
關(guān)鍵詞 浙貝母;配方顆粒;指紋圖譜;高效液相色譜法;含量測定
Fingerprint Establishment and Content Determination of 3 Components in Fritillaria thunbergii Formula Granules
HUANG Xiaolan1,2,HE Xufeng1,ZHOU Nong2,YANG Wenwu1,QIAN Linqun2(1. Chongqing Wanzhou Food and Drug Inspection Institute, Chongqing 404100, China; 2. College of Food and Biological Engineering/Chongqing Engineering Laboratory for Green Cultivation and Deep Processing of the Three Gorges Reservoir Areas Medicinal Herbs, Chongqing Three Gorges University, Chongqing 404100, China)
ABSTRACT? ?OBJECTIVE: To establish the fingerprint of Fritillariae thunbergii formula granules and determine the contents of 3 components. METHODS: HPLC method was used. Using peiminine as reference, HPLC fingerprints of 13 batches of F. thunbergii formula granules were drawn with Similarity Evaluation System of TCM Chromatogram Fingerprint(2012 edition). Similarity evaluation and common peak identification were conducted. The contents of peimisine, peimine and peiminine in F. thunbergii formula granules were determined by the same HPLC method. The quality difference of samples were compared among different manufacturers. RESULTS: There were 5 common peaks in 13 batches of F. thunbergii formula granules, and the similarity was 0.669-0.971. Three common peaks of peimisine, peimine and peiminine were identified. The linear ranges of peimisine, peimine and peiminine were 30.00-180.00 μg/mL (r=0.999 9), 79.58-477.50 μg/mL (r=0.999 6) and 97.33-584.00 μg/mL (r=0.999 4), respectively. RSDs of precision, stability (24 h) and reproducibility tests were all lower than 3%. The average recoveries were 95.82% (RSD=1.17%,n=6), 99.00%(RSD=1.96%,n=6) and 95.39%(RSD=2.00%,n=6), respectively. In the 13 batches of samples, the content of peimisine, peimine and peiminine were 0.17-1.02 mg/g, 0.52-2.26 mg/g, and 0.70-3.50 mg/g, respectively. Their average total content was 3.62 mg/g. The average total content of manufacturer C and A was higher (5.02 mg/g and 4.61 mg/g), followed by manufacturer E and B (3.48 mg/g and 3.02 mg/g); the lowest was manufacturer D (only 1.87 mg/g). CONCLUSIONS: Established fingerprint and content determination method is simple, feasible and reproducible, which can be used for the quality evaluation of F. thunbergii formula granules. There are some differences in content among different manu- facturers.