西北药学杂志
西北藥學雜誌
서북약학잡지
2015年
4期
364-366,367
,共4页
李莉%王佳宇%高山山%侯文珍%马长华
李莉%王佳宇%高山山%侯文珍%馬長華
리리%왕가우%고산산%후문진%마장화
聚山梨酯80%挥发性杂质%气相色谱法
聚山梨酯80%揮髮性雜質%氣相色譜法
취산리지80%휘발성잡질%기상색보법
polysorbate 80%volatile impurities%gas chromatography
目的:建立气相色谱法对聚山梨酯80中的环氧乙烷、二氧六环、氯乙醇、乙二醇和二甘醇5种挥发性杂质进行同时检测。方法采用气相色谱法,色谱柱固定相为PEG20000(GsBP‐INOWAX ,30 m ×0.53 mm ×1.0μm弹性石英毛细管柱)。采用程序升温,初温50℃,以5℃· min-1升温至200℃,保持10 min ,再以50℃· min-1升温至230℃,保持20 min。进样口温度为200℃,检测器温度为250℃。结果同时测定了聚山梨酯80中环氧乙烷、二氧六环、氯乙醇、乙二醇和二甘醇5种挥发性杂质,线性范围分别为2.7~176.8μg·mL -1(r=0.9998),2.8~140.7μg·mL-1(r=0.9998),3.4~167.5μg·mL-1(r=0.9999),4.7~2345μg·mL -1(r=0.9998)和3.2~160.8μg·mL -1(r=0.9999);平均加样回收率分别为104.3%,91.3%,105.2%,94.1%和105.7%,RSD分别为2.5%,2.8%,1.4%,3.0%和3.7%。结论该方法灵敏、准确,可用于聚山梨酯80中挥发性杂质的检测。
目的:建立氣相色譜法對聚山梨酯80中的環氧乙烷、二氧六環、氯乙醇、乙二醇和二甘醇5種揮髮性雜質進行同時檢測。方法採用氣相色譜法,色譜柱固定相為PEG20000(GsBP‐INOWAX ,30 m ×0.53 mm ×1.0μm彈性石英毛細管柱)。採用程序升溫,初溫50℃,以5℃· min-1升溫至200℃,保持10 min ,再以50℃· min-1升溫至230℃,保持20 min。進樣口溫度為200℃,檢測器溫度為250℃。結果同時測定瞭聚山梨酯80中環氧乙烷、二氧六環、氯乙醇、乙二醇和二甘醇5種揮髮性雜質,線性範圍分彆為2.7~176.8μg·mL -1(r=0.9998),2.8~140.7μg·mL-1(r=0.9998),3.4~167.5μg·mL-1(r=0.9999),4.7~2345μg·mL -1(r=0.9998)和3.2~160.8μg·mL -1(r=0.9999);平均加樣迴收率分彆為104.3%,91.3%,105.2%,94.1%和105.7%,RSD分彆為2.5%,2.8%,1.4%,3.0%和3.7%。結論該方法靈敏、準確,可用于聚山梨酯80中揮髮性雜質的檢測。
목적:건립기상색보법대취산리지80중적배양을완、이양륙배、록을순、을이순화이감순5충휘발성잡질진행동시검측。방법채용기상색보법,색보주고정상위PEG20000(GsBP‐INOWAX ,30 m ×0.53 mm ×1.0μm탄성석영모세관주)。채용정서승온,초온50℃,이5℃· min-1승온지200℃,보지10 min ,재이50℃· min-1승온지230℃,보지20 min。진양구온도위200℃,검측기온도위250℃。결과동시측정료취산리지80중배양을완、이양륙배、록을순、을이순화이감순5충휘발성잡질,선성범위분별위2.7~176.8μg·mL -1(r=0.9998),2.8~140.7μg·mL-1(r=0.9998),3.4~167.5μg·mL-1(r=0.9999),4.7~2345μg·mL -1(r=0.9998)화3.2~160.8μg·mL -1(r=0.9999);평균가양회수솔분별위104.3%,91.3%,105.2%,94.1%화105.7%,RSD분별위2.5%,2.8%,1.4%,3.0%화3.7%。결론해방법령민、준학,가용우취산리지80중휘발성잡질적검측。
Objective To establish a method for the determination of five volatile impurities in polysorbate 80 .Method The determi‐nation was performed on a GsBP‐INOWAX column with PEG20000(30 m × 0 .53 mm × 1 .0 μm) as solid phase .The column tem‐peratures was 50 ℃ at beginning ,and programmed to 200 ℃ at a rate of 5 ℃ · min-1 ,maintained for 10 min;then programmed to 230 ℃ at a rate of 50 ℃ · min-1 and held for 20 min .The temperatures of the injector and detector were set at 200 and 250 ℃ , respectively .Result Five volatile impurities in polysorbate 80 were determined simultaneously by gas chromatography .The calibration curves were linear in the ranges of 2 .7‐176 .8 μg · mL -1 (r=0 .999 8) ,2 .8‐140 .7 μg · mL -1 (r=0 .999 8) ,3 .4‐167 .5 μg · mL -1 (r=0 .999 9) ,4 .7‐2 345 μg · mL -1 (r=0 .999 8) ,and 3 .2‐160 .8 μg · mL -1 (r=0 .999 9) for ethylene oxide ,dioxane ,ethylene chlorohydrin ,ethylene glycol and diethylene glycol ,respectively .The average recoveries were 104 .3% ,91 .3% ,105 .2% ,94 .1%and 105 .7% ,RSD were 2 .5% ,2 .8% ,1 .4% ,3 .0% and 3 .7% ,respectively .Conclusion The method were proved to be accurate and sensitive ,and can be used for the detection of the volatile impurities in polysorbate 80 .