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
4251-4257
,共7页
卢高超%王小娟%李红光%穆登峰%刘永健
盧高超%王小娟%李紅光%穆登峰%劉永健
로고초%왕소연%리홍광%목등봉%류영건
高效液相色谱-串联质谱法%加热电喷雾电离%豆芽%4-氯苯氧乙酸钠
高效液相色譜-串聯質譜法%加熱電噴霧電離%豆芽%4-氯苯氧乙痠鈉
고효액상색보-천련질보법%가열전분무전리%두아%4-록분양을산납
high performance liquid chromatography-tandem mass spectrometry%heating-electrospray ionization%bean sprouts%sodium parachlorophenoxy
目的:建立豆芽中4-氯苯氧乙酸钠的液相色谱-串联质谱测定方法。方法豆芽样品均质后以0.01 mol/L氢氧化钠溶液提取,提取液经酸化后再用乙酸乙酯萃取,收集经离心分层的有机相,浓缩后用甲醇溶解进行测定分析。以甲醇和0.1%甲酸(FA)水溶液为流动相,采用Hypersil GOLD aQ (100 mm×2.1 mm,3μm)色谱柱分离,电喷雾电离负离子条件下以选择反应监测模式(SRM)检测。结果该方法检出限0.005 mg/kg,在1~100 ng/mL范围内具有良好线性,相关系数为0.9998。回收率为79.1%~104.7%,相对标准偏差低于5%(n=6)。结论该方法前处理简单快速,定性准确,灵敏度好,适用于豆芽中4-氯苯氧乙酸钠的残留检测。
目的:建立豆芽中4-氯苯氧乙痠鈉的液相色譜-串聯質譜測定方法。方法豆芽樣品均質後以0.01 mol/L氫氧化鈉溶液提取,提取液經痠化後再用乙痠乙酯萃取,收集經離心分層的有機相,濃縮後用甲醇溶解進行測定分析。以甲醇和0.1%甲痠(FA)水溶液為流動相,採用Hypersil GOLD aQ (100 mm×2.1 mm,3μm)色譜柱分離,電噴霧電離負離子條件下以選擇反應鑑測模式(SRM)檢測。結果該方法檢齣限0.005 mg/kg,在1~100 ng/mL範圍內具有良好線性,相關繫數為0.9998。迴收率為79.1%~104.7%,相對標準偏差低于5%(n=6)。結論該方法前處理簡單快速,定性準確,靈敏度好,適用于豆芽中4-氯苯氧乙痠鈉的殘留檢測。
목적:건립두아중4-록분양을산납적액상색보-천련질보측정방법。방법두아양품균질후이0.01 mol/L경양화납용액제취,제취액경산화후재용을산을지췌취,수집경리심분층적유궤상,농축후용갑순용해진행측정분석。이갑순화0.1%갑산(FA)수용액위류동상,채용Hypersil GOLD aQ (100 mm×2.1 mm,3μm)색보주분리,전분무전리부리자조건하이선택반응감측모식(SRM)검측。결과해방법검출한0.005 mg/kg,재1~100 ng/mL범위내구유량호선성,상관계수위0.9998。회수솔위79.1%~104.7%,상대표준편차저우5%(n=6)。결론해방법전처리간단쾌속,정성준학,령민도호,괄용우두아중4-록분양을산납적잔류검측。
Objective To establish a method for determination of sodium parachlorophenoxy (4-CPANa) in bean sprouts by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). MethodsThe soybean sample was extracted with 0.01 mol/L sodium hydroxide solution, and the extracting solution was recovered by diethyl ether in acidic condition. After centrifugation, the organic phase was concentrated completely and re-dissolved with methanol. The sample was separated by a Hypersil GOLD aQ column (100 mm×2.1 mm, 3μm) with methanol and 0.1% FA aqueous as mobile phase. The remnant was detected by MS/MS using H-ESI technology (negative ion mode) and SRM detection mode.ResultsThe detection limit was 0.005 mg/kg and the linear range was 1~100 ng/mL with correlation coefficient (r2) of 0.9998. The average recoveries were between 79.1%~104.7% with relative standard deviation (RSD) less than 5% (n=6).ConclusionThisanalytical method is sample, rapid, accurate, and sensitive, and can be used for the rapid detection of sodium parachlorophenoxy in bean sprouts.