中国中医药信息杂志
中國中醫藥信息雜誌
중국중의약신식잡지
CHINESE JOURNAL OF INFORMATION ON TRADITIONAL CHINESE MEDICINE
2013年
12期
46-48
,共3页
邢俊波%曹红%张炯%单婷婷%水彩红%陈玉敏%胡丹
邢俊波%曹紅%張炯%單婷婷%水綵紅%陳玉敏%鬍丹
형준파%조홍%장형%단정정%수채홍%진옥민%호단
柱前衍生化%低分子羰基化合物%高效液相色谱法%2,4-二硝基苯肼
柱前衍生化%低分子羰基化閤物%高效液相色譜法%2,4-二硝基苯肼
주전연생화%저분자탄기화합물%고효액상색보법%2,4-이초기분정
pro-column derivatization%low-molecular-weight carbonyl compounds%HPLC%2,4-dinitrophenylhydrazine
目的:建立高效液相色谱法(HPLC)测定含油脂类药材中低分子羰基化合物的方法。方法苦杏仁等药材经水提取,在酸性条件下,经2,4-二硝基苯肼(DNPH)衍生后,衍生物直接用HPLC测定。色谱柱:Kromasil KR100-5 C18(250 mm×4.6 mm,5μm);流动相:A为水-乙腈-四氢呋南-异丙醇(59∶30∶10∶1),B为水-乙腈(35∶65),梯度洗脱;流速:0.8 mL/min;检测波长:365 nm;柱温:30℃。结果甲醛、乙醛、丙酮、丙烯醛、丙醛、巴豆醛、2-丁酮、丁醛的DNPH衍生物在一定浓度范围内与峰面积线性关系良好,相关系数均达到0.999以上,平均回收率为88.49%~93.65%,最低检测限为0.002~0.008μg/mL。结论该方法简便、灵敏、准确、重复性较好。
目的:建立高效液相色譜法(HPLC)測定含油脂類藥材中低分子羰基化閤物的方法。方法苦杏仁等藥材經水提取,在痠性條件下,經2,4-二硝基苯肼(DNPH)衍生後,衍生物直接用HPLC測定。色譜柱:Kromasil KR100-5 C18(250 mm×4.6 mm,5μm);流動相:A為水-乙腈-四氫呋南-異丙醇(59∶30∶10∶1),B為水-乙腈(35∶65),梯度洗脫;流速:0.8 mL/min;檢測波長:365 nm;柱溫:30℃。結果甲醛、乙醛、丙酮、丙烯醛、丙醛、巴豆醛、2-丁酮、丁醛的DNPH衍生物在一定濃度範圍內與峰麵積線性關繫良好,相關繫數均達到0.999以上,平均迴收率為88.49%~93.65%,最低檢測限為0.002~0.008μg/mL。結論該方法簡便、靈敏、準確、重複性較好。
목적:건립고효액상색보법(HPLC)측정함유지류약재중저분자탄기화합물적방법。방법고행인등약재경수제취,재산성조건하,경2,4-이초기분정(DNPH)연생후,연생물직접용HPLC측정。색보주:Kromasil KR100-5 C18(250 mm×4.6 mm,5μm);류동상:A위수-을정-사경부남-이병순(59∶30∶10∶1),B위수-을정(35∶65),제도세탈;류속:0.8 mL/min;검측파장:365 nm;주온:30℃。결과갑철、을철、병동、병희철、병철、파두철、2-정동、정철적DNPH연생물재일정농도범위내여봉면적선성관계량호,상관계수균체도0.999이상,평균회수솔위88.49%~93.65%,최저검측한위0.002~0.008μg/mL。결론해방법간편、령민、준학、중복성교호。
Objective To establish an HPLC method for determination of low-molecular-weight carbonyl compounds in the oil-containing herbs. Methods After carbonyl compounds in the samples were extracted with water, the solution reacted with 2, 4-dinitrophenylhydrazine (DNPH) in an acidic medium to form 2, 4-dinitrophenylhydrazone derivatives, which were separated on Kromasil KR100-5 C18 column (250 mm× 4.6 mm, 5 μm). The mobile phase A was water-acetonitrile-tetrahydrofuran-isopropanol (59∶30∶10∶1), mobile phase B was water-acetonitrile (35∶65), gradient elution. The flow rate was 0.8 mL/min, detection wavelength was 365 nm, and column temperature was 30 ℃. Results Good linearities were obtained in corresponding concentration ranges, with correlation coefficient over 0.999. The limits of detection of the eight DNPH derivatives were 0.002-0.008 μg/mL, and the average recoveries were 88.49%-93.65%. Conclusion The method is simple, accurate and reliable, with good reproducibility.