生物医学工程研究
生物醫學工程研究
생물의학공정연구
JOURNAL OF BIOMEDICAL ENGINEERING RESEARCH
2015年
2期
106-109
,共4页
刘阳%马丽霞%王勤%王传栋%冯圣玉
劉暘%馬麗霞%王勤%王傳棟%馮聖玉
류양%마려하%왕근%왕전동%풍골옥
聚乳酸%封端剂%气相色谱法%氢离子火焰检测器
聚乳痠%封耑劑%氣相色譜法%氫離子火燄檢測器
취유산%봉단제%기상색보법%경리자화염검측기
Poly (lactic acid )%Endcapper%gas chromatography (GC )%Hydrogen flame ionization detector (FID )
建立了一种气相色谱法测定聚乳酸原料中封端剂十二醇残留的分析方法。着重研究了测定方法及样品的预处理方法。实验结果显示,采用 DB -624(30m ×0.530mm ×3.0μm)毛细管柱,氢火焰离子检测器,进样口温度250℃,检测器温度260℃,程序升温(起始温度60℃,维持3 min,以30℃/min 的速率升温至250℃,维持10min),十二醇的回归方程为 A =2717.3C -11.646(γ=0.9998),线性范围为0.01~1.01 mg/mL,平均回收率为99.21%(n =9),相对标准偏差1.55%,检测限为0.0005 mg/mL,定量限为0.001 mg/mL。本实验所建立的方法能达到定量检测的目的,将该方法应用于聚乳酸原料中封端剂十二醇残留量的测定,结果可靠。
建立瞭一種氣相色譜法測定聚乳痠原料中封耑劑十二醇殘留的分析方法。著重研究瞭測定方法及樣品的預處理方法。實驗結果顯示,採用 DB -624(30m ×0.530mm ×3.0μm)毛細管柱,氫火燄離子檢測器,進樣口溫度250℃,檢測器溫度260℃,程序升溫(起始溫度60℃,維持3 min,以30℃/min 的速率升溫至250℃,維持10min),十二醇的迴歸方程為 A =2717.3C -11.646(γ=0.9998),線性範圍為0.01~1.01 mg/mL,平均迴收率為99.21%(n =9),相對標準偏差1.55%,檢測限為0.0005 mg/mL,定量限為0.001 mg/mL。本實驗所建立的方法能達到定量檢測的目的,將該方法應用于聚乳痠原料中封耑劑十二醇殘留量的測定,結果可靠。
건립료일충기상색보법측정취유산원료중봉단제십이순잔류적분석방법。착중연구료측정방법급양품적예처리방법。실험결과현시,채용 DB -624(30m ×0.530mm ×3.0μm)모세관주,경화염리자검측기,진양구온도250℃,검측기온도260℃,정서승온(기시온도60℃,유지3 min,이30℃/min 적속솔승온지250℃,유지10min),십이순적회귀방정위 A =2717.3C -11.646(γ=0.9998),선성범위위0.01~1.01 mg/mL,평균회수솔위99.21%(n =9),상대표준편차1.55%,검측한위0.0005 mg/mL,정량한위0.001 mg/mL。본실험소건립적방법능체도정량검측적목적,장해방법응용우취유산원료중봉단제십이순잔류량적측정,결과가고。
A gas chromatography method was developed for the determination of lauryl alcohol residual in poly (lactic acid ).It focused on studying the gas chromatography method and the pretreatment method of PLA.The result of the experiment showed that a DB -624 column (30m ×0.53mm ×3.0μm)was adopted,the inlet temperature was controlled at 250 ℃ and the FID detector tem-perature was 260 ℃,the oven temperature was initially held at 60 ℃ for 3 min and was then programmed to 250 ℃ at 30 ℃/min and held for another 10 min,the linearity equation of lauryl alcohol was A =2717.3C -11.646 (γ=0.9998),the linear range was 0.01 mg/mL ~1.01mg/mL,and the average recovery was 99.21% (n =9),the RSD was 1.55%,the limit of detection was 0.0005 mg/mL.The limit of quantification was 0.001mg/mL,the method can achieve the purpose of lauryl alcohol quantitative detection.The analysis of lauryl alcohol residual in poly (lactic acid)verify the reliability of this method.