光谱学与光谱分析
光譜學與光譜分析
광보학여광보분석
SPECTROSCOPY AND SPECTRAL ANALYSIS
2014年
9期
2568-2572
,共5页
张春娟%孟志芬%郭雪峰%岳永德%汤锋%喻谨%陈超
張春娟%孟誌芬%郭雪峰%嶽永德%湯鋒%喻謹%陳超
장춘연%맹지분%곽설봉%악영덕%탕봉%유근%진초
黄酮碳苷%HPLC%紫外光谱%荭草苷%异荭草苷%牡荆苷%异牡荆苷
黃酮碳苷%HPLC%紫外光譜%葒草苷%異葒草苷%牡荊苷%異牡荊苷
황동탄감%HPLC%자외광보%홍초감%이홍초감%모형감%이모형감
Flavone C-glycosides%HPLC-UV%Orientin%Isoorientin%Vitexin%Isovitexin
采用 HPLC结合紫外光谱法,同时测定四种竹叶黄酮碳苷(荭草苷、异荭草苷、牡荆苷和异牡荆苷)。采用Waters XTerra MS C18色谱柱(250 mm ×4.6 mm ,5μm),流动相为乙腈和0.5%甲酸水溶液,等梯度洗脱,流速1 mL · min-1,柱温30℃,检测波长360 nm。建立各个组分在0.1~10.0 mg · L -1范围内系列浓度的混合标准工作曲线,其相关系数 R2均优于0.999,且在22 min内得到较好分离。方法检出限介于0.03~0.07 mg · L -1,定量限介于0.04~0.08 mg · L -1。分别将标准品与样品中四种黄酮碳苷的紫外光谱(240~400 nm )进行比对,荭草苷、异荭草苷、牡荆苷和异牡荆苷相应的光谱曲线形状以及特征吸收波长都表现出高吻合度。取竹叶样品经热回流提取,石油醚萃取及AB-8大孔树脂纯化后,再采用 HPLC结合紫外光谱法检测得荭草苷、异荭草苷、牡荆苷和异牡荆苷四种黄酮碳苷相对于竹叶黄酮粉的百分含量分别为13.73,49.68,7.85和30.70 mg · g -1,平均回收率为34.90%~87.64%,相对标准偏差为0.41%~10.83%。本方法实现了在较短时间内快速分析竹叶中四种黄酮碳苷,样品稳定,重现性好,为市售竹叶黄酮碳苷的质量控制提供参考。
採用 HPLC結閤紫外光譜法,同時測定四種竹葉黃酮碳苷(葒草苷、異葒草苷、牡荊苷和異牡荊苷)。採用Waters XTerra MS C18色譜柱(250 mm ×4.6 mm ,5μm),流動相為乙腈和0.5%甲痠水溶液,等梯度洗脫,流速1 mL · min-1,柱溫30℃,檢測波長360 nm。建立各箇組分在0.1~10.0 mg · L -1範圍內繫列濃度的混閤標準工作麯線,其相關繫數 R2均優于0.999,且在22 min內得到較好分離。方法檢齣限介于0.03~0.07 mg · L -1,定量限介于0.04~0.08 mg · L -1。分彆將標準品與樣品中四種黃酮碳苷的紫外光譜(240~400 nm )進行比對,葒草苷、異葒草苷、牡荊苷和異牡荊苷相應的光譜麯線形狀以及特徵吸收波長都錶現齣高吻閤度。取竹葉樣品經熱迴流提取,石油醚萃取及AB-8大孔樹脂純化後,再採用 HPLC結閤紫外光譜法檢測得葒草苷、異葒草苷、牡荊苷和異牡荊苷四種黃酮碳苷相對于竹葉黃酮粉的百分含量分彆為13.73,49.68,7.85和30.70 mg · g -1,平均迴收率為34.90%~87.64%,相對標準偏差為0.41%~10.83%。本方法實現瞭在較短時間內快速分析竹葉中四種黃酮碳苷,樣品穩定,重現性好,為市售竹葉黃酮碳苷的質量控製提供參攷。
채용 HPLC결합자외광보법,동시측정사충죽협황동탄감(홍초감、이홍초감、모형감화이모형감)。채용Waters XTerra MS C18색보주(250 mm ×4.6 mm ,5μm),류동상위을정화0.5%갑산수용액,등제도세탈,류속1 mL · min-1,주온30℃,검측파장360 nm。건립각개조분재0.1~10.0 mg · L -1범위내계렬농도적혼합표준공작곡선,기상관계수 R2균우우0.999,차재22 min내득도교호분리。방법검출한개우0.03~0.07 mg · L -1,정량한개우0.04~0.08 mg · L -1。분별장표준품여양품중사충황동탄감적자외광보(240~400 nm )진행비대,홍초감、이홍초감、모형감화이모형감상응적광보곡선형상이급특정흡수파장도표현출고문합도。취죽협양품경열회류제취,석유미췌취급AB-8대공수지순화후,재채용 HPLC결합자외광보법검측득홍초감、이홍초감、모형감화이모형감사충황동탄감상대우죽협황동분적백분함량분별위13.73,49.68,7.85화30.70 mg · g -1,평균회수솔위34.90%~87.64%,상대표준편차위0.41%~10.83%。본방법실현료재교단시간내쾌속분석죽협중사충황동탄감,양품은정,중현성호,위시수죽협황동탄감적질량공제제공삼고。
High-performance liquid chromatography with ultraviolet spectrometer (HPLC-UV) was used to simultaneously de-tect the four flavone C-glycosides ,i .e .orientin ,isoorientin ,vitexin and isovitexin .Analytes were separated with Waters XTer-ra MS C18 column (250 mm × 4.6 mm ,5 μm) using acetonitrile and 0.5% (φ) formic acid as mobile phase .The flow rate was set at 1.0 mL · min-1 with the column temperature at 30 ℃ ,and the detection wavelength was 360 nm .The calibration curve was linear over the concentration range of 0.1~10.0 mg · L -1 for the mixed standard solution .Analytes were separated in 22 minutes ,and the relative standard deviation values were all above 0.999 .LOD values of standards were found to be between 0.03 and 0.07 mg · L -1 ,and LOQ values were in the range of 0.04~0.08 mg · L -1 .After comparing the spectra (240~400 nm) of four flavone C-glycosides in mixed standards and the final product purified by macroporous resin ,respectively ,the curve shape and characteristic ultraviolet absorption wavelength of each flavone C-glycoside including orientin ,isoorientin ,vitexin and isovitexin were fitted well .The bamboo leaves sample was extracted by ethanol under reflux ,and then partitioned with water and petroleum ether .The aqueous phase was added onto macroporous resin(AB-8) ,and the fraction of ethanol-water (40% ,φ) was concentrated .It was found that the contents of orientin ,isoorientin ,vitexin and isovitexin relative to the fraction of ethanol-water were 13.73 ,49.68 ,7.85 and 30.70 mg · g -1 ,respectively .In addition ,the average recovery of the four flavone C-glyco-sides ranged from 34.90% to 87.64% with RSD values from 0.41% to 10.83% .The results showed that bamboo leaves sample had good stability and repeatability .The new method was used to analyze the four flavone C-glycosides quickly and provide quali-ty control for commercial products .