分析测试学报
分析測試學報
분석측시학보
JOURNAL OF INSTRUMENTAL ANALYSIS
2010年
1期
55-58
,共4页
林子俺%庞纪磊%黄慧%郑江南%张兰
林子俺%龐紀磊%黃慧%鄭江南%張蘭
림자엄%방기뢰%황혜%정강남%장란
毛细管电泳%水产品%己烷雌酚%己烯雌酚%双烯雌酚
毛細管電泳%水產品%己烷雌酚%己烯雌酚%雙烯雌酚
모세관전영%수산품%기완자분%기희자분%쌍희자분
capillary electrophoresis%aquatic product%hexestrol%diethylstibestrol%dienestrol
建立了毛细管电泳-紫外检测法测定水产品中己烷雌酚(HXS)、己烯雌酚(DES)及双烯雌酚(DIES)残留的新方法.研究了缓冲体系的酸度、浓度、添加剂、分离电压、进样时间及温度等对组分分离的影响.在检测波长为200 nm,分离电压为20 kV,运行缓冲液为50 mmol/L硼砂-25 mmol/L氢氧化纳(pH 12.3,含30%的N,N-二甲基甲酰胺)的条件下,3种目标组分在14 min内达到基线分离.HXS、DES 与DIES 的质量浓度与峰面积分别在2.0 ~120、1.0 ~100、1.0 ~100 mg/L范围内呈良好线性,相关系数(r~2)分别为0.999 8、0.999 2、0.999 4,检出限为0.3 ~0.9 mg/L.将该方法用于鲫鱼中3种雌酚类激素的检测,结果令人满意.
建立瞭毛細管電泳-紫外檢測法測定水產品中己烷雌酚(HXS)、己烯雌酚(DES)及雙烯雌酚(DIES)殘留的新方法.研究瞭緩遲體繫的痠度、濃度、添加劑、分離電壓、進樣時間及溫度等對組分分離的影響.在檢測波長為200 nm,分離電壓為20 kV,運行緩遲液為50 mmol/L硼砂-25 mmol/L氫氧化納(pH 12.3,含30%的N,N-二甲基甲酰胺)的條件下,3種目標組分在14 min內達到基線分離.HXS、DES 與DIES 的質量濃度與峰麵積分彆在2.0 ~120、1.0 ~100、1.0 ~100 mg/L範圍內呈良好線性,相關繫數(r~2)分彆為0.999 8、0.999 2、0.999 4,檢齣限為0.3 ~0.9 mg/L.將該方法用于鯽魚中3種雌酚類激素的檢測,結果令人滿意.
건립료모세관전영-자외검측법측정수산품중기완자분(HXS)、기희자분(DES)급쌍희자분(DIES)잔류적신방법.연구료완충체계적산도、농도、첨가제、분리전압、진양시간급온도등대조분분리적영향.재검측파장위200 nm,분리전압위20 kV,운행완충액위50 mmol/L붕사-25 mmol/L경양화납(pH 12.3,함30%적N,N-이갑기갑선알)적조건하,3충목표조분재14 min내체도기선분리.HXS、DES 여DIES 적질량농도여봉면적분별재2.0 ~120、1.0 ~100、1.0 ~100 mg/L범위내정량호선성,상관계수(r~2)분별위0.999 8、0.999 2、0.999 4,검출한위0.3 ~0.9 mg/L.장해방법용우즉어중3충자분류격소적검측,결과령인만의.
A facile method was developed for simultaneous determination of hexestrol(HXS),diethylstibestrol(DES) and dienestrol(DIES) residues in aquatic product based on capillary electrophoresis coupled with ultraviolet detection.The influences of some important factors such as additive,acidity and concentration of running buffer,separation voltage,injection time and temperature were systemically investigated.At the detection wavelength of 200 nm,a good baseline separation of three analytes was obtained within 14 min by using 50 mmol/L borax-25 mmol/L NaOH(pH 12.3) with additive of 30%(by volume) DMF as running buffer and 20 kV as an applied voltage.The calibration curves were linear in the range of 2.0-120 mg/L for HXS and 1.0-100 mg/L for DES and DIES,with correlation coefficients of 0.999 8,0.999 2 and 0.999 4,respectively.The limits of detection(S/N=3) of HXS,DES and DIES were 0.9,0.4 and 0.3 mg/L,respectively.The average recoveries from samples at spiked concentration level of 50 mg/L were ranged from 92% to 98% with RSDs of 2.3% -3.9%.The method showed a good repeatability and high sensitivity,and was applied in the determination of three analytes in real sample with satisfactory result.