哈尔滨医科大学学报
哈爾濱醫科大學學報
합이빈의과대학학보
JOURNAL OF HARBIN MEDICAL UNIVERSITY
2015年
2期
95-98,102
,共5页
杨异卉%陈卫军%甘春丽%王立波%吴立军%陈华昌
楊異卉%陳衛軍%甘春麗%王立波%吳立軍%陳華昌
양이훼%진위군%감춘려%왕립파%오립군%진화창
戒酒灵口服液%葫芦素B%葫芦素E%薄层色谱%高效液相色谱法
戒酒靈口服液%葫蘆素B%葫蘆素E%薄層色譜%高效液相色譜法
계주령구복액%호호소B%호호소E%박층색보%고효액상색보법
JIE JIU LING oral liquid%cucurbitacin B%cucurbitacin E%TLC%HPLC
目的:建立戒酒灵口服液中葫芦素B和葫芦素E的TLC鉴别和HPLC含量测定的方法,为建立戒酒灵口服液质量标准提供参考。方法采用TLC法对戒酒灵口服液中葫芦素B和葫芦素E进行定性鉴别,并采用HPLC法对二者进行含量测定。色谱条件:COSMOSIL C18色谱柱(250 mm ×4.6 mm,5μm);乙腈(A)和0.2%醋酸-水溶液(B)梯度洗脱(0.0~15.0 min:30%~40% A;15.0~40.0 min:40%~45%A);检测波长为234 nm;柱温为室温;流速为1 mL/min;进样量为10μL。结果在TLC图中,戒酒灵口服液的供试品溶液分别与葫芦素B、E的对照品溶液在相同位置上显现暗斑。含量测定实验中,葫芦素B和葫芦素E质量浓度分别在0.01574~0.3148 mg/mL和0.003744~0.07488 mg/mL范围内与峰面积呈良好的线性关系,平均回收率分别为97.7%(RSD=1.29%,n=6)和98.4%(RSD=1.68%,n=6)。戒酒灵口服液中葫芦素B和葫芦素E的平均含量分别为0.36 mg/mL( RSD=0.85%,n=6)和0.033 mg/mL( RSD=0.78%,n=6)。结论此鉴别和含量测定方法简便、快捷、准确、可靠,能有效地对戒酒灵口服液的质量进行控制。
目的:建立戒酒靈口服液中葫蘆素B和葫蘆素E的TLC鑒彆和HPLC含量測定的方法,為建立戒酒靈口服液質量標準提供參攷。方法採用TLC法對戒酒靈口服液中葫蘆素B和葫蘆素E進行定性鑒彆,併採用HPLC法對二者進行含量測定。色譜條件:COSMOSIL C18色譜柱(250 mm ×4.6 mm,5μm);乙腈(A)和0.2%醋痠-水溶液(B)梯度洗脫(0.0~15.0 min:30%~40% A;15.0~40.0 min:40%~45%A);檢測波長為234 nm;柱溫為室溫;流速為1 mL/min;進樣量為10μL。結果在TLC圖中,戒酒靈口服液的供試品溶液分彆與葫蘆素B、E的對照品溶液在相同位置上顯現暗斑。含量測定實驗中,葫蘆素B和葫蘆素E質量濃度分彆在0.01574~0.3148 mg/mL和0.003744~0.07488 mg/mL範圍內與峰麵積呈良好的線性關繫,平均迴收率分彆為97.7%(RSD=1.29%,n=6)和98.4%(RSD=1.68%,n=6)。戒酒靈口服液中葫蘆素B和葫蘆素E的平均含量分彆為0.36 mg/mL( RSD=0.85%,n=6)和0.033 mg/mL( RSD=0.78%,n=6)。結論此鑒彆和含量測定方法簡便、快捷、準確、可靠,能有效地對戒酒靈口服液的質量進行控製。
목적:건립계주령구복액중호호소B화호호소E적TLC감별화HPLC함량측정적방법,위건립계주령구복액질량표준제공삼고。방법채용TLC법대계주령구복액중호호소B화호호소E진행정성감별,병채용HPLC법대이자진행함량측정。색보조건:COSMOSIL C18색보주(250 mm ×4.6 mm,5μm);을정(A)화0.2%작산-수용액(B)제도세탈(0.0~15.0 min:30%~40% A;15.0~40.0 min:40%~45%A);검측파장위234 nm;주온위실온;류속위1 mL/min;진양량위10μL。결과재TLC도중,계주령구복액적공시품용액분별여호호소B、E적대조품용액재상동위치상현현암반。함량측정실험중,호호소B화호호소E질량농도분별재0.01574~0.3148 mg/mL화0.003744~0.07488 mg/mL범위내여봉면적정량호적선성관계,평균회수솔분별위97.7%(RSD=1.29%,n=6)화98.4%(RSD=1.68%,n=6)。계주령구복액중호호소B화호호소E적평균함량분별위0.36 mg/mL( RSD=0.85%,n=6)화0.033 mg/mL( RSD=0.78%,n=6)。결론차감별화함량측정방법간편、쾌첩、준학、가고,능유효지대계주령구복액적질량진행공제。
Objective To establish an effective TLC and HPLC method for qualitative and quantitative analysis of cucurbitacin B and cucurbitacin E in JIE JIU LING oral liquid , which can be used to control the quality of JIE JIU LING oral liquid .Methods Cucurbitacin B and cucurbitacin E in JIE JIU LING oral liquid were identified and determined by TLC and HPLC . The conditions of HPLC included the column of COSMOSIL C 18 column (250 mm ×4.6 mm, 5 μm), the mobile phase of acetonitrile-0.2%acetic acid solution (0.0~15.0 min:30%~40%A;15.0~40.0 min:40%~45% A) , a flow rate of 1.0 mL/min, the detection wave-length of 234 nm.Results In contrast to the control solution of cucurbitacin B and cucurbita-cin E, the sample solution of JIE JIU LING oral liquid appeared dark spots in the same position of TLC, respectively .The linear ranges of cucurbitacin B and cucurbitacin E were 0.015 74~0.314 8 mg/mL and 0.003 744~0.074 88 mg/mL, respectively .The average recovery of cu-curbitacin B and cucurbitacin E were 97.7% ( RSD=1.29%, n=6 ) and 98.4% ( RSD=1.68%, n=6), respectively.The average content of cucurbitacin B and cucurbitacin E in JIE JIU LING oral liquid were 0.36 mg/mL ( RSD=0.85%, n=6 ) and 0.033mg /mL ( RSD=0.78%, n=6), respectively.Conclusion The methods of TLC and HPLC are reliable, sta-ble and repeatable , which can be applied as the quantity control method of cucurbitacin B and cucurbitacin E in JIE JIU LING oral liquid .