饲料工业
飼料工業
사료공업
FEED INDUSTRY
2013年
15期
51-53
,共3页
饲料%加速溶剂萃取%固相萃取%气相色谱-质谱%三聚氰胺
飼料%加速溶劑萃取%固相萃取%氣相色譜-質譜%三聚氰胺
사료%가속용제췌취%고상췌취%기상색보-질보%삼취청알
feed%accelerated solvent extraction%solid-phase extraction%GC/MS%melamine
研究旨在建立一种饲料中三聚氰胺残留测定的加速溶剂萃取-固相萃取-气相色谱-质谱方法。饲料样品经加速溶剂萃取仪提取,固相萃取净化后,气相色谱-质谱法(GC-MS)测定。筛选并优化了饲料中三聚氰胺残留的提取试剂、提取方法,确定了加速溶剂萃取仪工作条件,筛选了高效、适用的色谱柱,并确定了色谱、质谱条件。结果表明,加速溶剂萃取方法对阳性样品的提取效果显著优于超声萃取法,选用甲醇水溶液(V:V=1:4)替代腐蚀性较强的10%三氯乙酸溶液,萃取效果好且不易腐蚀加速溶剂萃取仪,HP-5MS色谱柱分离效果优于DB-35MS色谱柱。采用本方法,提取效率高,且方法简便、快速,能满足饲料中三聚氰胺残留检测的需要,显著优于NY/T 1372-2007《饲料中三聚氰胺的测定》标准中采用的超声萃取法。
研究旨在建立一種飼料中三聚氰胺殘留測定的加速溶劑萃取-固相萃取-氣相色譜-質譜方法。飼料樣品經加速溶劑萃取儀提取,固相萃取淨化後,氣相色譜-質譜法(GC-MS)測定。篩選併優化瞭飼料中三聚氰胺殘留的提取試劑、提取方法,確定瞭加速溶劑萃取儀工作條件,篩選瞭高效、適用的色譜柱,併確定瞭色譜、質譜條件。結果錶明,加速溶劑萃取方法對暘性樣品的提取效果顯著優于超聲萃取法,選用甲醇水溶液(V:V=1:4)替代腐蝕性較彊的10%三氯乙痠溶液,萃取效果好且不易腐蝕加速溶劑萃取儀,HP-5MS色譜柱分離效果優于DB-35MS色譜柱。採用本方法,提取效率高,且方法簡便、快速,能滿足飼料中三聚氰胺殘留檢測的需要,顯著優于NY/T 1372-2007《飼料中三聚氰胺的測定》標準中採用的超聲萃取法。
연구지재건립일충사료중삼취청알잔류측정적가속용제췌취-고상췌취-기상색보-질보방법。사료양품경가속용제췌취의제취,고상췌취정화후,기상색보-질보법(GC-MS)측정。사선병우화료사료중삼취청알잔류적제취시제、제취방법,학정료가속용제췌취의공작조건,사선료고효、괄용적색보주,병학정료색보、질보조건。결과표명,가속용제췌취방법대양성양품적제취효과현저우우초성췌취법,선용갑순수용액(V:V=1:4)체대부식성교강적10%삼록을산용액,췌취효과호차불역부식가속용제췌취의,HP-5MS색보주분리효과우우DB-35MS색보주。채용본방법,제취효솔고,차방법간편、쾌속,능만족사료중삼취청알잔류검측적수요,현저우우NY/T 1372-2007《사료중삼취청알적측정》표준중채용적초성췌취법。
A method by gas chromatography-mass spectrometry determination of melamine in feed by accelerated solvent extraction purify coupled with solid-phase extraction cleanup after detective condition was optimized. The work condition of accelerated solvent extractor and gas chromatography-mass spectrometry were confirmed and the method of extraction cleanup were optimized. The experiment demonstrated that accelerated extraction to be better than ultrasound-assisted extraction in detecting positive samples of melamine. And the methanol solution(V:V=1:4)is more suitable for extraction melamine in feed than that of trimethoxy silaneacetic acid, it also showed that the HP-5MS chromatographic column was superior to DB-35MS column in the determination of melamine in feed. The method is easy to operate, and with good precision, it is therefore well suited for the routine determination of melamine in feed samples.