中山大学学报(自然科学版)
中山大學學報(自然科學版)
중산대학학보(자연과학판)
ACTA SCIENTIARUM NATURALIUM UNIVERSITATIS SUNYATSENI
2013年
6期
104-109
,共6页
邢丽红%冷凯良%孙伟红%翟毓秀%李兆新%谭志军%苗钧魁
邢麗紅%冷凱良%孫偉紅%翟毓秀%李兆新%譚誌軍%苗鈞魁
형려홍%랭개량%손위홍%적육수%리조신%담지군%묘균괴
气相色谱法%鱼%虾%复硝酚钠%残留
氣相色譜法%魚%蝦%複硝酚鈉%殘留
기상색보법%어%하%복초분납%잔류
Gas chromatography%fish%shrimp%sodium nitrophenolate%residue
样品用乙酸乙酯提取、酸性氧化铝去脂、碳酸钾溶液反萃取、乙酸酐衍生后,正己烷萃取衍生产物,气相色谱-ECD检测器测定,外标法定量。结果表明:3种化合物在5~100μg/L范围内线性关系良好,相关系数R2>0.999,检测限为5μg/kg,对硝基酚钠的回收率为86.4%~89.6%,邻硝基酚钠的回收率为82.8%~84.3%,2-甲氧基-5-硝基苯酚钠的回收率为89.9%~92.2%,相对标准偏差均<15%。该方法适用于鱼和虾可食部分中复硝酚钠的常规残留检测。
樣品用乙痠乙酯提取、痠性氧化鋁去脂、碳痠鉀溶液反萃取、乙痠酐衍生後,正己烷萃取衍生產物,氣相色譜-ECD檢測器測定,外標法定量。結果錶明:3種化閤物在5~100μg/L範圍內線性關繫良好,相關繫數R2>0.999,檢測限為5μg/kg,對硝基酚鈉的迴收率為86.4%~89.6%,鄰硝基酚鈉的迴收率為82.8%~84.3%,2-甲氧基-5-硝基苯酚鈉的迴收率為89.9%~92.2%,相對標準偏差均<15%。該方法適用于魚和蝦可食部分中複硝酚鈉的常規殘留檢測。
양품용을산을지제취、산성양화려거지、탄산갑용액반췌취、을산항연생후,정기완췌취연생산물,기상색보-ECD검측기측정,외표법정량。결과표명:3충화합물재5~100μg/L범위내선성관계량호,상관계수R2>0.999,검측한위5μg/kg,대초기분납적회수솔위86.4%~89.6%,린초기분납적회수솔위82.8%~84.3%,2-갑양기-5-초기분분납적회수솔위89.9%~92.2%,상대표준편차균<15%。해방법괄용우어화하가식부분중복초분납적상규잔류검측。
After the samples were extracted by ethyl acetate,the supernatant were cleansed by acidic a-lumina and extracted by potassium carbonate.The extracts were then reacted with acetic anhydride.The products were detected by gas chromatography with ECD detector via an external standard method follow-ing being extracted by n-hexane.The linearity of three compounds were held in 5 ~1 00 μg/L,with cor-relation coefficient R2 >0.999 .The detection limits for the GC method (S/N=3 )of the nitrophenolate were 5 μg/kg.The tests for recovery were carried by addition of standard at concentration of 1 0 ~1 00μg/kg.The result indicated that the residue content of p-nitrophenol sodium,o-nitrophenol sodium and 2-methoxy-5-nitropenolate sodium were 86.4% ~89.6%,82.8% ~84.3% and 89.9% ~92.2%, respectively,while the relative standard deviations were less than 1 5%.This method can be used to de-termine the residue content of nitrophenolate in edible portion of fish and shrimp.