粮油加工（电子版）
糧油加工（電子版）
량유가공（전자판）
Cereals and Oils Processing（Electronic Version）
2014年
6期
47-49
,共3页
苏红伟%赵华锋%周嘉明%罗司玉
囌紅偉%趙華鋒%週嘉明%囉司玉
소홍위%조화봉%주가명%라사옥
灭瘟素%残留%糙米%亲水作用液相色谱-质谱/质谱
滅瘟素%殘留%糙米%親水作用液相色譜-質譜/質譜
멸온소%잔류%조미%친수작용액상색보-질보/질보
Blasticidin-S%Residue%Brown rice%Hydrophilic interaction liquid chromatography-mass spec-trometry/mass spectrometry (HILIC-MS/MS)
建立了糙米中灭瘟素残留量的亲水作用液相色谱-质谱联用测定方法。样品用80%甲醇/水提取，经MCX 固相萃取小柱净化，以Waters HPLC BEH HILIC 色谱柱（100mm×2.1mm，1.7μm）分离，采用 U鄄PLC-MS/MS 多反应监测（MRM）正离子模式测定，外标法定量。灭瘟素最低检测浓度为0.02mg/kg，在0.02、0.05和0.20mg/kg 3个添加水平下平均回收率为78%～95%，相对标准偏差为2.9%～5.2%。
建立瞭糙米中滅瘟素殘留量的親水作用液相色譜-質譜聯用測定方法。樣品用80%甲醇/水提取，經MCX 固相萃取小柱淨化，以Waters HPLC BEH HILIC 色譜柱（100mm×2.1mm，1.7μm）分離，採用 U鄄PLC-MS/MS 多反應鑑測（MRM）正離子模式測定，外標法定量。滅瘟素最低檢測濃度為0.02mg/kg，在0.02、0.05和0.20mg/kg 3箇添加水平下平均迴收率為78%～95%，相對標準偏差為2.9%～5.2%。
건립료조미중멸온소잔류량적친수작용액상색보-질보련용측정방법。양품용80%갑순/수제취，경MCX 고상췌취소주정화，이Waters HPLC BEH HILIC 색보주（100mm×2.1mm，1.7μm）분리，채용 U견PLC-MS/MS 다반응감측（MRM）정리자모식측정，외표법정량。멸온소최저검측농도위0.02mg/kg，재0.02、0.05화0.20mg/kg 3개첨가수평하평균회수솔위78%～95%，상대표준편차위2.9%～5.2%。
A method of determination for blasticidin-S in brown rice by HILIC-MS/MS was established. Analytes were extracted from samples using methanol and water ( V/V, 8∶2) , and purified with MCX solid phase extraction columns, then analyzed using UPLC-MS/MS multiple reaction monitoring (MRM) mode via positive electrospray ion-ization with a Waters HPLC BEH HILIC column (100mm×2.1mm, 1.7μm) as the analytical column. All analytes were quantified by external standard method. Limit of quantification was 0.02mg/kg. Results showed that average recoveries at fortified levels of 0.02, 0.05 and 0.2 mg/kg ranged from 78%to 95%, and RSD were 2.9%-5.2%.
