福建农业学报
福建農業學報
복건농업학보
FUJIAN JOURNAL OF AGRICULTURAL SCIENCES
2014年
10期
987-994
,共8页
王丽丽%陈键%宋振硕%陈林
王麗麗%陳鍵%宋振碩%陳林
왕려려%진건%송진석%진림
茶叶%HPLC%没食子酸%儿茶素类%生物碱
茶葉%HPLC%沒食子痠%兒茶素類%生物堿
다협%HPLC%몰식자산%인다소류%생물감
tea%HPLC%gallic acid%catechins%alkaloids
比较 ZorbaxSB-C18与 TSKgelODS-100Z这2种色谱柱对12个组分的分离效果,从洗脱方式、流动相pH 值、柱温与流速等方面优化色谱条件,并对其进行方法学考查以及茶样测定应用,从而建立了一种同时测定茶叶中没食子酸(GA)、8种儿茶素类(GC、EGC、C、EGCG、EC、GCG、ECG、CG)与3种生物碱(可可碱、茶碱、咖啡碱)的高效液相色谱(HPLC)检测方法。确立的最优色谱条件为:采用 TSKgelODS-100Z (4.6mm×150mm,5μm)色谱柱,流动相为2‰甲酸水溶液(A 相)和甲醇(B相),洗脱方式为83%A (0 min)→75%A (5min)→73%A (7min)→58%A (16min)→83%A (18min),柱温为40℃,流速为1.0mL ·min-1,检测波长为280nm。茶叶中各组分回归方程的相关系数均在0.9990以上,保留时间与峰面积的精密度RSD 分别小于0.105%与4.076%,加标回收率在97.767%~104.766%。该方法具有良好的线性关系、精密度和回收率,对待测组分的分离效果好,适用于茶叶中没食子酸、儿茶素类及生物碱含量的准确测定。
比較 ZorbaxSB-C18與 TSKgelODS-100Z這2種色譜柱對12箇組分的分離效果,從洗脫方式、流動相pH 值、柱溫與流速等方麵優化色譜條件,併對其進行方法學攷查以及茶樣測定應用,從而建立瞭一種同時測定茶葉中沒食子痠(GA)、8種兒茶素類(GC、EGC、C、EGCG、EC、GCG、ECG、CG)與3種生物堿(可可堿、茶堿、咖啡堿)的高效液相色譜(HPLC)檢測方法。確立的最優色譜條件為:採用 TSKgelODS-100Z (4.6mm×150mm,5μm)色譜柱,流動相為2‰甲痠水溶液(A 相)和甲醇(B相),洗脫方式為83%A (0 min)→75%A (5min)→73%A (7min)→58%A (16min)→83%A (18min),柱溫為40℃,流速為1.0mL ·min-1,檢測波長為280nm。茶葉中各組分迴歸方程的相關繫數均在0.9990以上,保留時間與峰麵積的精密度RSD 分彆小于0.105%與4.076%,加標迴收率在97.767%~104.766%。該方法具有良好的線性關繫、精密度和迴收率,對待測組分的分離效果好,適用于茶葉中沒食子痠、兒茶素類及生物堿含量的準確測定。
비교 ZorbaxSB-C18여 TSKgelODS-100Z저2충색보주대12개조분적분리효과,종세탈방식、류동상pH 치、주온여류속등방면우화색보조건,병대기진행방법학고사이급다양측정응용,종이건립료일충동시측정다협중몰식자산(GA)、8충인다소류(GC、EGC、C、EGCG、EC、GCG、ECG、CG)여3충생물감(가가감、다감、가배감)적고효액상색보(HPLC)검측방법。학립적최우색보조건위:채용 TSKgelODS-100Z (4.6mm×150mm,5μm)색보주,류동상위2‰갑산수용액(A 상)화갑순(B상),세탈방식위83%A (0 min)→75%A (5min)→73%A (7min)→58%A (16min)→83%A (18min),주온위40℃,류속위1.0mL ·min-1,검측파장위280nm。다협중각조분회귀방정적상관계수균재0.9990이상,보류시간여봉면적적정밀도RSD 분별소우0.105%여4.076%,가표회수솔재97.767%~104.766%。해방법구유량호적선성관계、정밀도화회수솔,대대측조분적분리효과호,괄용우다협중몰식자산、인다소류급생물감함량적준학측정。
Using HPLC,an analytical method was developed to simultaneously determine the contents of gallic acid(GA),8 catechins (i.e.,GC,EGC,C,EGCG,EC,GCG,ECG and CG)and 3 alkaloids (i .e.,theobromine,theophylline and caffeine)in tea.Separation of the 1 2 chemicals on two chromatographic columns (Zorbax SB-C1 8and TSKgel ODS-1 00Z ) were investigated. The chromatographic conditions applied were the result fromoptimizations of the elution mode,pH of the mobile phase,column temperature and flow rate.They included:maintaining TSKgel ODS-1 00Z column at 40℃,using 2 ‰ formic acid-water solution (mobile phase A )andmethanol (mobile phase B)with the gradient elution mode of 83 % A (0 min)→7 5 % A (5 min) →7 3 % A (7min)→5 8% A (16min)→83 % A (18min)at the flow rate of 1.0 mL·min-1 ,and detecting at the wavelength of 280nm.Methodological evaluation and application on 6 tea samples were subsequently conducted for verification.Thecorrelation coefficients of the resulting linear equations for all of the components were greater than 0.9 9 90,RSDs %of accuracy of the retention time and peak area lower than 0.1 05 % and 4.07 6 %,respectively,and the recoveryrates from 9 7.7 6 7 % to 1 04.7 6 6 %.It appeared that the newly developed analytical method could yield linearrelationships on data,as well as desirable precision,recovery and separability on the measurements for accurate andsimultaneous determinations of gallic acid,catechins and alkaloids in tea.