中山大学学报（自然科学版）
中山大學學報（自然科學版）
중산대학학보（자연과학판）
ACTA SCIENTIARUM NATURALIUM UNIVERSITATIS SUNYATSENI
2014年
1期
89-92
,共4页
林惠贞%刘浩文%韦玮%李雯婷%赵志敏%陈建萍%王冬梅
林惠貞%劉浩文%韋瑋%李雯婷%趙誌敏%陳建萍%王鼕梅
림혜정%류호문%위위%리문정%조지민%진건평%왕동매
鸡血藤%密花豆属密花豆%原儿茶酸%高效液相色谱法
鷄血籐%密花豆屬密花豆%原兒茶痠%高效液相色譜法
계혈등%밀화두속밀화두%원인다산%고효액상색보법
Spatholobi Caulis%Spatholobus suberectus%protocatechuic acid%HPLC
建立测定鸡血藤药材中原儿茶酸含量的方法，并对制备供试品溶液的提取溶剂、提取方法、提取次数、药材粒度等进行了考察优化。采用高效液相色谱法，色谱柱：Diamonsil C18色谱柱（250×4.6 mm，5μm）；流动相为乙腈-φ＝0.5％醋酸水（体积比为10∶90）；流速为1.0 mL·min-1；检测波长为260 nm。优化所得供试品溶液的制备方法，药材加水回流提取3次，每次1.5 h，合并提取液并浓缩至小体积，用乙酸乙酯萃取4次，合并乙酸乙酯萃取液，浓缩后的残渣用甲醇-水（体积比为1∶1）溶解并定容，即得。经系统的方法学考察，所建立的方法在原儿茶酸浓度为8.56～214μg·mL-1范围内线性良好（R2＝0.9997），平均加样回收率为99.2％， RSD为2.8％，市售7个批次鸡血藤药材中原儿茶酸的含量为65.81～122.35μg·g-1。该方法准确，重复性好，可用于鸡血藤药材的质量控制。
建立測定鷄血籐藥材中原兒茶痠含量的方法，併對製備供試品溶液的提取溶劑、提取方法、提取次數、藥材粒度等進行瞭攷察優化。採用高效液相色譜法，色譜柱：Diamonsil C18色譜柱（250×4.6 mm，5μm）；流動相為乙腈-φ＝0.5％醋痠水（體積比為10∶90）；流速為1.0 mL·min-1；檢測波長為260 nm。優化所得供試品溶液的製備方法，藥材加水迴流提取3次，每次1.5 h，閤併提取液併濃縮至小體積，用乙痠乙酯萃取4次，閤併乙痠乙酯萃取液，濃縮後的殘渣用甲醇-水（體積比為1∶1）溶解併定容，即得。經繫統的方法學攷察，所建立的方法在原兒茶痠濃度為8.56～214μg·mL-1範圍內線性良好（R2＝0.9997），平均加樣迴收率為99.2％， RSD為2.8％，市售7箇批次鷄血籐藥材中原兒茶痠的含量為65.81～122.35μg·g-1。該方法準確，重複性好，可用于鷄血籐藥材的質量控製。
건립측정계혈등약재중원인다산함량적방법，병대제비공시품용액적제취용제、제취방법、제취차수、약재립도등진행료고찰우화。채용고효액상색보법，색보주：Diamonsil C18색보주（250×4.6 mm，5μm）；류동상위을정-φ＝0.5％작산수（체적비위10∶90）；류속위1.0 mL·min-1；검측파장위260 nm。우화소득공시품용액적제비방법，약재가수회류제취3차，매차1.5 h，합병제취액병농축지소체적，용을산을지췌취4차，합병을산을지췌취액，농축후적잔사용갑순-수（체적비위1∶1）용해병정용，즉득。경계통적방법학고찰，소건립적방법재원인다산농도위8.56～214μg·mL-1범위내선성량호（R2＝0.9997），평균가양회수솔위99.2％， RSD위2.8％，시수7개비차계혈등약재중원인다산적함량위65.81～122.35μg·g-1。해방법준학，중복성호，가용우계혈등약재적질량공제。
High performance liquid chromatography (HPLC)was developed for the quantitative analysis of protocatechuic acid (PA)in Spatholobi Caulis (the stem of Suberect spatholobus Dunn.).The prepa-ration method of sample solution was established by optimizing the extraction solvents,methods,times and the sizes of the crude drug.The sample solutions were analyzed using a C18 column (250 ×4.6 mm,5μm)with CH3 CN-φ=0.5%HAc (volumic ratio,10∶90)as mobile phase and detected at 260 nm with a flow rate of 1.0 mL·min-1 .The crude drug was extracted by boiling water for three times and 1.5 h for each time.The obtained aqueous solution was concentrated and followed by extracted with ethyl acetate for four times.The ethyl acetate layer was concentrated to dryness,and was resolved in methanol-water (volumic ratio,1∶1 )to give the sample solution previous to HPLC analysis.After systematic method evaluation,the results showed that the linear range was 8.56 ~214 μg·mL-1 with correlation coefficient R2 of 0.999 7;and the average recovery rate was 99.2%with RSD of 2.8%.The contents of PA in market-sold seven batches of Spatholobi Caulis were determined to be in the range of 65.8 1 ~122.35 μg·g-1.The established method was accurate and repeatable,which could be used for the quality control of Spatholobi Caulis.
