广东化工
廣東化工
엄동화공
GUANGDONG CHEMICAL INDUSTRY
2012年
8期
148-150
,共3页
付尽国%孟飞%陈骏佳%徐晓燕
付儘國%孟飛%陳駿佳%徐曉燕
부진국%맹비%진준가%서효연
高效液相色谱%蒸发光散射检测器%甘油%二聚甘油%三聚甘油
高效液相色譜%蒸髮光散射檢測器%甘油%二聚甘油%三聚甘油
고효액상색보%증발광산사검측기%감유%이취감유%삼취감유
HPLC%ELSD%glycerol%diglycerol%triglycerol
建立了高效液相色谱-蒸发光散射检测器(HPLC-ELSD)测定低聚甘油组成的方法。以Econosphere Amino(250×4.6 mm,5μm)为色谱柱,乙腈-水(85∶15,V/V)为流动相,流速为1.0 mL/min,柱温为28℃,进样量为30μL,ELSD漂移管温度为32℃,载气流速为1.5 L/min。结果表明,在优化条件下,甘油、二聚甘油和三聚甘油浓度分别在100~300μg/mL、100~400μg/mL和200~600μg/mL范围内呈良好线性,相关系数分别为0.9979、0.9921和0.9969,定量下限分别为1.5、1.0和2.0μg,回收率为97%~103%,RSD〈3.0%(n=6)。
建立瞭高效液相色譜-蒸髮光散射檢測器(HPLC-ELSD)測定低聚甘油組成的方法。以Econosphere Amino(250×4.6 mm,5μm)為色譜柱,乙腈-水(85∶15,V/V)為流動相,流速為1.0 mL/min,柱溫為28℃,進樣量為30μL,ELSD漂移管溫度為32℃,載氣流速為1.5 L/min。結果錶明,在優化條件下,甘油、二聚甘油和三聚甘油濃度分彆在100~300μg/mL、100~400μg/mL和200~600μg/mL範圍內呈良好線性,相關繫數分彆為0.9979、0.9921和0.9969,定量下限分彆為1.5、1.0和2.0μg,迴收率為97%~103%,RSD〈3.0%(n=6)。
건립료고효액상색보-증발광산사검측기(HPLC-ELSD)측정저취감유조성적방법。이Econosphere Amino(250×4.6 mm,5μm)위색보주,을정-수(85∶15,V/V)위류동상,류속위1.0 mL/min,주온위28℃,진양량위30μL,ELSD표이관온도위32℃,재기류속위1.5 L/min。결과표명,재우화조건하,감유、이취감유화삼취감유농도분별재100~300μg/mL、100~400μg/mL화200~600μg/mL범위내정량호선성,상관계수분별위0.9979、0.9921화0.9969,정량하한분별위1.5、1.0화2.0μg,회수솔위97%~103%,RSD〈3.0%(n=6)。
An analytical method was established for the determination of the composition of oligoglycerols by using HPLC with ELSD.The optimal conditions were as follows: column was Econosphere Amino(250×4.6 mm,5 μm),mobile phase: mixture of acetonitrile and water(85:15),flow rate: 1.0 mL/min,column temperature: 28 ℃,injection volume: 30 μL,drift tube temperature: 32 ℃,flow rate of carrier gas: 1.5 L/min.Under the optimal conditions,the calibration curve was linear over the content of glycerol,diglycerol and triglycerol in the range of 100~300 μg/mL,100~400 μg/mL and 200~600 μg/mL with a correlation coefficient of 0.9979,0.9921 and 0.9969,the limit of quantification(S/N≥10) were 1.5,1.0 and 2.0 μg.The spiked recoveries were in the range of 97 %~103 % with relative standard deviations(RSDs)3.0 %(n=6).