CAJ | 학술논문

采用大蒜新素键合硅胶固定相(DTSP),建立了一种同时测定人尿中5-氟尿嘧啶、5-溴尿嘧啶、5-碘尿嘧啶、磺胺嘧啶和磺胺二甲嘧啶的高效液相色谱方法.以甲醇-0.01 mol·L-1NaH2PO4缓冲液(30:70,ν/ν,pH 3.0)为流动相,流速为0.8 mL·min-1,操作柱温为30 ℃,二极管阵列检测器监测,定量波长为254 nm.研究发现,大蒜新素固定相能较好地分离上述五种嘧啶类化合物,并用于模拟人尿液样品的定量分析.结果表明,它们的浓度与峰面积呈现良好的线性关系,线性范围分别依次为:1～50 μg·mL-1,r=0.999 6;5～45 μg·mL-1,r=0.999 6;5～45 μg·mL-1,r=0.999 8;5～45 μg·mL-1,r=0.999 8;5～45 μg·mL-1,r=0.999 9.平均回收率分别为:99.59%,99.43%,100.6%,98.32%,97.94%.本方法前处理简便、灵敏度和选择性较好.
채용대산신소건합규효고정상(DTSP),건립료일충동시측정인뇨중5-불뇨밀정、5-추뇨밀정、5-전뇨밀정、광알밀정화광알이갑밀정적고효액상색보방법.이갑순-0.01 mol·L-1NaH2PO4완충액(30:70,ν/ν,pH 3.0)위류동상,류속위0.8 mL·min-1,조작주온위30 ℃,이겁관진렬검측기감측,정량파장위254 nm.연구발현,대산신소고정상능교호지분리상술오충밀정류화합물,병용우모의인뇨액양품적정량분석.결과표명,타문적농도여봉면적정현량호적선성관계,선성범위분별의차위:1～50 μg·mL-1,r=0.999 6;5～45 μg·mL-1,r=0.999 6;5～45 μg·mL-1,r=0.999 8;5～45 μg·mL-1,r=0.999 8;5～45 μg·mL-1,r=0.999 9.평균회수솔분별위:99.59%,99.43%,100.6%,98.32%,97.94%.본방법전처리간편、령민도화선택성교호.
An HPLC method for determination of five pyrimidines,such as 5-fluorouracil,5-bromouracil,5-iodouracil,sulfadiazine and sulfamethazine on diallyl trisulfide-bonded stationary phase (DTSP) was first developed by HPLC.Chromatographic analysis was carried out by using methanol-0.01 mol·L-1NaH2PO4(30:70,ν/ν,pH 3.0) as mobile phase at a flowed of 0.8mL/min with DAD detector at 254nm under 30℃.The results showed that the better separation of the above pyrimidines on DTSP could be achieved than that of ODS.Some spiked human urines were analyzed in this experiment.The good linearity was observed.Their linear ranges were 1～50 μgmL-1,5～45 μgmL-1,5～45 μgmL-1,5～45 μgmL-1 and 5～45 μgmL-1,respectively.The average recoveries were separately 99.59%,99.43%,100.6%,98.32% and 97.94%.The method was simple for pretreatment,accurate and reliable for quantification of five pyrimidines in human urine within 20 min.