中华预防医学杂志
中華預防醫學雜誌
중화예방의학잡지
CHINESE JOURNAL OF
2012年
8期
750-753
,共4页
邱文倩%刘晓霞%郑奎城%傅武胜
邱文倩%劉曉霞%鄭奎城%傅武勝
구문천%류효하%정규성%부무성
红曲霉属%色谱法,亲和%色谱法,高压液相%桔青霉素
紅麯黴屬%色譜法,親和%色譜法,高壓液相%桔青黴素
홍곡매속%색보법,친화%색보법,고압액상%길청매소
Monascus%Chromatography,affinity%Chromatography,high pressure liquid%Citrinin
目的 建立红曲产品中桔青霉素的免疫亲和层析净化( I C) -高效液相色谱(HPLC)检测方法,检测福建相关红曲产品中桔青霉素(CIT)的含量.方法 采用I C-HPLC的方法对红曲产品中CIT的含量进行测定.HPLC的条件为:色谱柱:C18反相色谱柱,150.0 mm×4.6 mm×3μm；流动相:采用乙腈和体积分数为0.1％磷酸溶液,体积比值为65:35,等度洗脱；柱温:28℃；流速:0.8 ml/min;荧光检测器波长:激发光波长(λex)为331 nm、发射光波长(λem)为500 nm.根据峰面积(Y)对CIT浓度(X,ng/ml)进行线性回归,绘制标准曲线,并验证方法的准确度和精密度.采用建立的方法对32种福建红曲产品进行测定和色价比较.结果 本研究建立方法的标准曲线为Y =4634.8X - 136.42,r=1.000,最低检测限为20μg/kg,定量限为64 μg/kg.在200～ 800 μg/kg范围内,加标同收率为98.9％～110.0％(n=3),RSD为0.51％～1.76％.32份样品中,11份红曲米、9份红曲粉和5份红曲色素均检测出CIT,含量为0.212 ～ 14.500 mg/kg,7份功能性红曲中有4份检出CIT,含量为0.142 ～0.275 mg/kg.结论 建立I C-HPLC法测定红曲产品中CIT的方法.
目的 建立紅麯產品中桔青黴素的免疫親和層析淨化( I C) -高效液相色譜(HPLC)檢測方法,檢測福建相關紅麯產品中桔青黴素(CIT)的含量.方法 採用I C-HPLC的方法對紅麯產品中CIT的含量進行測定.HPLC的條件為:色譜柱:C18反相色譜柱,150.0 mm×4.6 mm×3μm；流動相:採用乙腈和體積分數為0.1％燐痠溶液,體積比值為65:35,等度洗脫；柱溫:28℃；流速:0.8 ml/min;熒光檢測器波長:激髮光波長(λex)為331 nm、髮射光波長(λem)為500 nm.根據峰麵積(Y)對CIT濃度(X,ng/ml)進行線性迴歸,繪製標準麯線,併驗證方法的準確度和精密度.採用建立的方法對32種福建紅麯產品進行測定和色價比較.結果 本研究建立方法的標準麯線為Y =4634.8X - 136.42,r=1.000,最低檢測限為20μg/kg,定量限為64 μg/kg.在200～ 800 μg/kg範圍內,加標同收率為98.9％～110.0％(n=3),RSD為0.51％～1.76％.32份樣品中,11份紅麯米、9份紅麯粉和5份紅麯色素均檢測齣CIT,含量為0.212 ～ 14.500 mg/kg,7份功能性紅麯中有4份檢齣CIT,含量為0.142 ～0.275 mg/kg.結論 建立I C-HPLC法測定紅麯產品中CIT的方法.
목적 건립홍곡산품중길청매소적면역친화층석정화( I C) -고효액상색보(HPLC)검측방법,검측복건상관홍곡산품중길청매소(CIT)적함량.방법 채용I C-HPLC적방법대홍곡산품중CIT적함량진행측정.HPLC적조건위:색보주:C18반상색보주,150.0 mm×4.6 mm×3μm；류동상:채용을정화체적분수위0.1％린산용액,체적비치위65:35,등도세탈；주온:28℃；류속:0.8 ml/min;형광검측기파장:격발광파장(λex)위331 nm、발사광파장(λem)위500 nm.근거봉면적(Y)대CIT농도(X,ng/ml)진행선성회귀,회제표준곡선,병험증방법적준학도화정밀도.채용건립적방법대32충복건홍곡산품진행측정화색개비교.결과 본연구건립방법적표준곡선위Y =4634.8X - 136.42,r=1.000,최저검측한위20μg/kg,정량한위64 μg/kg.재200～ 800 μg/kg범위내,가표동수솔위98.9％～110.0％(n=3),RSD위0.51％～1.76％.32빈양품중,11빈홍곡미、9빈홍곡분화5빈홍곡색소균검측출CIT,함량위0.212 ～ 14.500 mg/kg,7빈공능성홍곡중유4빈검출CIT,함량위0.142 ～0.275 mg/kg.결론 건립I C-HPLC법측정홍곡산품중CIT적방법.
Objective To establish a method to test citrinin (CIT) in monascus products by immuno-affinity chromatography ( IAC)- high performance liquid chromatography ( HPLC ),and to detect the content of CIT in monascus products in Fujian province.Methods IAC-HPLC was applied to detect the CIT content in monascus products.The conditions to use HPLC were as follows: C18 reversed-phase chromatographic column,150.0 mm × 4.6mm × 3 μm; mobile phase:the volume ratio of acetonitrile and 0.1％ phosphoric acid solution at 65∶ 35; isocratic elution; column temperature:28 ℃; flow velocity:0.8 ml/min; fluorescence detector,excitation wavelength ( λex ) was 331 nm and emission wavelength ( λem )was 500 nm.The standard curved was established by the linear regression of peak area (Y) to CIT content (X,ng/ml).The accuracy and preeision of the method would then be verified.And 32 kinds of monascus products were determined and their color values were compared by this method.Result The standard curve established in this study was Y =4634.8X - 136.42,r =1.000; whose limits of detection was 20 μg/kg and the limits of qualification was 64 μg/kg.In the range between 200 and 800 μg/kg,the standard recovery rate was 98.9％ - 110.0％ ( n =3 ),and the relative standard deviation ( RSD ) was 0.51％ - 1.76％.Out of the 32 samples,CIT was detected from 11 samples of monascus rice,9 samples of monascus powder and 5 samples of monascus pigments,the content was around 0.212 - 14.500 mg/kg.4 out of 7 functional monascus samples were detected out CIT,whose content at 0.142 -0.275 mg/kg.Conclusion The method to detect CIT in monascus products by IAC-HPLC has been established.
