贵州农业科学
貴州農業科學
귀주농업과학
GUIZHOU AGRICULTURAL SCIENCES
2014年
11期
58-61
,共4页
曹国琼%张永萍%徐剑%高莉%廖小刚
曹國瓊%張永萍%徐劍%高莉%廖小剛
조국경%장영평%서검%고리%료소강
化风丹%乌头碱%新乌头碱%次乌头碱%高效液相色谱
化風丹%烏頭堿%新烏頭堿%次烏頭堿%高效液相色譜
화풍단%오두감%신오두감%차오두감%고효액상색보
Huafeng pill%aconitine%mesaconitine%hypaconitine%HPLC
为更好地控制化风丹药母质量,建立高效液相色谱法同时测定化风丹药母中乌头碱、新乌头碱和次乌头碱含量。结果表明:同时测定化风丹中乌头碱、新乌头碱、次乌头碱的色谱条件为 Inertsil ODS-SP C18色谱柱(4.6 mm×250 mm,5μm),流动相乙腈-四氢呋喃(25∶15)A,0.1 mol/L 乙酸铵溶液(每1000 mL加冰醋酸0.5 mL)B,梯度洗脱(0~22 min,20%~23% A,22~40 min,23%~25% A),流速1.0 mL/min,柱温30℃,检测波长235 nm。在该条件下,乌头碱、新乌头碱、次乌头碱分别在0.258~1.548μg、0.322~1.932μg、0.280~1.680μg 呈良好的线性关系,平均回收率为98.64%(RSD 2.72%)、96.61%(RSD 1.15%)和98.80%(RSD 1.91%),该方法操作简便、准确、重复性好。
為更好地控製化風丹藥母質量,建立高效液相色譜法同時測定化風丹藥母中烏頭堿、新烏頭堿和次烏頭堿含量。結果錶明:同時測定化風丹中烏頭堿、新烏頭堿、次烏頭堿的色譜條件為 Inertsil ODS-SP C18色譜柱(4.6 mm×250 mm,5μm),流動相乙腈-四氫呋喃(25∶15)A,0.1 mol/L 乙痠銨溶液(每1000 mL加冰醋痠0.5 mL)B,梯度洗脫(0~22 min,20%~23% A,22~40 min,23%~25% A),流速1.0 mL/min,柱溫30℃,檢測波長235 nm。在該條件下,烏頭堿、新烏頭堿、次烏頭堿分彆在0.258~1.548μg、0.322~1.932μg、0.280~1.680μg 呈良好的線性關繫,平均迴收率為98.64%(RSD 2.72%)、96.61%(RSD 1.15%)和98.80%(RSD 1.91%),該方法操作簡便、準確、重複性好。
위경호지공제화풍단약모질량,건립고효액상색보법동시측정화풍단약모중오두감、신오두감화차오두감함량。결과표명:동시측정화풍단중오두감、신오두감、차오두감적색보조건위 Inertsil ODS-SP C18색보주(4.6 mm×250 mm,5μm),류동상을정-사경부남(25∶15)A,0.1 mol/L 을산안용액(매1000 mL가빙작산0.5 mL)B,제도세탈(0~22 min,20%~23% A,22~40 min,23%~25% A),류속1.0 mL/min,주온30℃,검측파장235 nm。재해조건하,오두감、신오두감、차오두감분별재0.258~1.548μg、0.322~1.932μg、0.280~1.680μg 정량호적선성관계,평균회수솔위98.64%(RSD 2.72%)、96.61%(RSD 1.15%)화98.80%(RSD 1.91%),해방법조작간편、준학、중복성호。
The content of aconitine,mesaconitine and hypaconitine in Huafeng pill was detected by HPLC to further control quality of Huafeng pill.The results showed that the chromatographic condition of detecting content of aconitine,mesaconitine and hypaconitine in Huafeng pill includes Inertsil ODS-SP C18 chromatographic column (4.6 mm× 250 mm,5 μm),gradient elution by mobile phase A:acetonitrile/tetrahydrofuran (25 ∶ 15)and mobile phase B:0.1 mol/L ammonium acetate (containing 0.5mL glacial acetic acid per 1000 mL),1.0 mL/min flow velocity,30℃ column temperature and 235nm determination wavelength.There is a good linear relation under the above-mentioned chromatographic condition when the content of aconitine,mesaconitine and hypaconitine is 0.258~ 1.548 μg,0.322~ 1.932 μg and 0.280~1.680 μg respectively.The average recovery rate of aconitine,mesaconitine and hypaconitine is 98.64 %(RSD 2.72 %),96.61 %(RSD 1.15 %)and 98.80 %(RSD 1.91 %)separately,which indicates that the detection method has the advantages of easy operation,accuracy and good repeatability.