分析试验室
分析試驗室
분석시험실
ANALYTICAL LABORATORY
2010年
1期
76-79
,共4页
李利军%郝学超%程昊%吴启涛
李利軍%郝學超%程昊%吳啟濤
리리군%학학초%정호%오계도
毛细管电泳%胶束扫集%三聚氰胺
毛細管電泳%膠束掃集%三聚氰胺
모세관전영%효속소집%삼취청알
Capillary electrophoresis%Sweeping micellar electrokinetic chromatography%Melamine
研究胶束在线扫集毛细管电泳法测定三聚氰胺的可行性, 结果表明, 与区带毛细管电泳相比, 胶束在线扫集毛细管电泳法富集倍数提高约60倍. 缓冲体系为140 mmol/L SDS+20 mmol/L NaH2PO4 (pH 2.20)+10%(体积分数)甲醇, 分离电压-18 kV, 进样时间30 s, 测量波长214 nm. 考察了SDS浓度、 pH、进样时间、运行电压等因素对分离测定的影响情况. 在优化条件下, 三聚氰胺在9 min时出峰, 峰面积RSD≤3.7%. 方法检出限、线性范围、相关系数分别为: 0.13 μg/mL、 0.50~32.0 μg/mL、 0.9997. 方法可用于奶粉中三聚氰胺的分离测定.
研究膠束在線掃集毛細管電泳法測定三聚氰胺的可行性, 結果錶明, 與區帶毛細管電泳相比, 膠束在線掃集毛細管電泳法富集倍數提高約60倍. 緩遲體繫為140 mmol/L SDS+20 mmol/L NaH2PO4 (pH 2.20)+10%(體積分數)甲醇, 分離電壓-18 kV, 進樣時間30 s, 測量波長214 nm. 攷察瞭SDS濃度、 pH、進樣時間、運行電壓等因素對分離測定的影響情況. 在優化條件下, 三聚氰胺在9 min時齣峰, 峰麵積RSD≤3.7%. 方法檢齣限、線性範圍、相關繫數分彆為: 0.13 μg/mL、 0.50~32.0 μg/mL、 0.9997. 方法可用于奶粉中三聚氰胺的分離測定.
연구효속재선소집모세관전영법측정삼취청알적가행성, 결과표명, 여구대모세관전영상비, 효속재선소집모세관전영법부집배수제고약60배. 완충체계위140 mmol/L SDS+20 mmol/L NaH2PO4 (pH 2.20)+10%(체적분수)갑순, 분리전압-18 kV, 진양시간30 s, 측량파장214 nm. 고찰료SDS농도、 pH、진양시간、운행전압등인소대분리측정적영향정황. 재우화조건하, 삼취청알재9 min시출봉, 봉면적RSD≤3.7%. 방법검출한、선성범위、상관계수분별위: 0.13 μg/mL、 0.50~32.0 μg/mL、 0.9997. 방법가용우내분중삼취청알적분리측정.
On-line sweeping micellar electrokinetic chromatography (sweeping-MEKC) and capillary zone electrophoresis (CZE) were used for the determination of melamine. Compared to CZE, the sensitivity was improved about 60 times by sweeping-MEKC. The buffer medium contains 140 mmol/L SDS+20 mmol/L NaH2PO4 (pH 2.20)+10% methanol, separation voltage was -18 kV, sample injection time was 30 s, and the samples were detected at 214 nm. The effect of SDS concentration, pH in background solution, sample injection time and applied voltage were optimized. Under the optimum conditions, the determination time was within 9 min with RSD of peak area less than 3.7%. The LOD was 0.13 μg/mL, calibration plot was linear in the range of 0.50~32.0 μg/mL with r≥0.9997. Furthermore, this proposed sweeping-MEKC method was applied to the detection of melamine in powdered milk with satisfactory results.