食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
Journal of Food Safety & Quality
2015年
10期
4205-4211
,共7页
王丽%邵金良%刘兴勇%林涛%陈心连%魏茂琼%汪禄祥
王麗%邵金良%劉興勇%林濤%陳心連%魏茂瓊%汪祿祥
왕려%소금량%류흥용%림도%진심련%위무경%왕록상
分散固相萃取%高效液相色谱法%三氯生%三氯卡班
分散固相萃取%高效液相色譜法%三氯生%三氯卡班
분산고상췌취%고효액상색보법%삼록생%삼록잡반
dispersive solid-phase extraction%high performance liquid chromatography%triclosan%triclocarban
目的:建立分散固相萃取-高效液相色谱法测定水果中三氯生及三氯卡班残留的新方法。方法样品采用乙腈溶液涡旋超声提取后,加入十八烷基键合硅胶吸附剂(C18)作为分散固相萃取净化剂进行净化(200 mg),用高效液相色谱法在278 nm处测定,采用PICKERING C8色谱柱(4.6 mm×250 mm i.d.,5μm),以甲醇:水(78:22,V:V)的溶液为流动相等度洗脱,流速1.2 mL/min。结果在最优检测条件下,各目标化合物的加标回收率为72.9%~104.4%,相对标准偏差在2.1%~9.1%之间。三氯生及三氯卡班的检出限分别为0.05和0.02 mg/kg,定量限分别为0.15和0.06 mg/kg。结论该方法分析快速、简便,适用于水果中三氯生及三氯卡班的测定。
目的:建立分散固相萃取-高效液相色譜法測定水果中三氯生及三氯卡班殘留的新方法。方法樣品採用乙腈溶液渦鏇超聲提取後,加入十八烷基鍵閤硅膠吸附劑(C18)作為分散固相萃取淨化劑進行淨化(200 mg),用高效液相色譜法在278 nm處測定,採用PICKERING C8色譜柱(4.6 mm×250 mm i.d.,5μm),以甲醇:水(78:22,V:V)的溶液為流動相等度洗脫,流速1.2 mL/min。結果在最優檢測條件下,各目標化閤物的加標迴收率為72.9%~104.4%,相對標準偏差在2.1%~9.1%之間。三氯生及三氯卡班的檢齣限分彆為0.05和0.02 mg/kg,定量限分彆為0.15和0.06 mg/kg。結論該方法分析快速、簡便,適用于水果中三氯生及三氯卡班的測定。
목적:건립분산고상췌취-고효액상색보법측정수과중삼록생급삼록잡반잔류적신방법。방법양품채용을정용액와선초성제취후,가입십팔완기건합규효흡부제(C18)작위분산고상췌취정화제진행정화(200 mg),용고효액상색보법재278 nm처측정,채용PICKERING C8색보주(4.6 mm×250 mm i.d.,5μm),이갑순:수(78:22,V:V)적용액위류동상등도세탈,류속1.2 mL/min。결과재최우검측조건하,각목표화합물적가표회수솔위72.9%~104.4%,상대표준편차재2.1%~9.1%지간。삼록생급삼록잡반적검출한분별위0.05화0.02 mg/kg,정량한분별위0.15화0.06 mg/kg。결론해방법분석쾌속、간편,괄용우수과중삼록생급삼록잡반적측정。
Objective To develop a method for determination of triclosan and triclocarban in fruit by dispersive solid-phase extraction (DSPE) combined with high performance liquid chromatography (HPLC). Methods The analytes were supersonic extracted from the fruit samples by acetonitrile, and purified by dispersion solid phase extraction using C18 sorbent (200 mg), then analyzed by high performance liquid chromatography with 278 nm detector. The chromatographic separation was performed on a PICKERING C8 column (4.6 mm×250 mm i.d., 5 μm), using a gradient elution program of methanol-H2O (78:22=V:V) as a mobile phase with a flow rate at 1.2 mL/min and the detector setting at 278 nm. Results Under optimization condition, the recoveries were in the range of 72.9%~104.4%, and the relative standard deviations (RSD) were 2.1%~9.1%. The limit of detection was 0.05 and 0.02 mg/kg, and the limit of quantification was 0.15 and 0.06 mg/kg for triclosan and triclocarban.ConclusionThis method was quick and easy, and applicable to determination of triclosan and triclocarban in fruit.