四川大学学报(医学版)
四川大學學報(醫學版)
사천대학학보(의학판)
JOURNAL OF WEST CHINA UNIVERSITY OF MEDICAL SCIENCES
2010年
1期
148-152
,共5页
何成艳%黎源倩%王慎骄%欧阳华学%郑波
何成豔%黎源倩%王慎驕%歐暘華學%鄭波
하성염%려원천%왕신교%구양화학%정파
浊点萃取%高效液相色谱法%二苯醚类除草剂%农药残留分析%水样
濁點萃取%高效液相色譜法%二苯醚類除草劑%農藥殘留分析%水樣
탁점췌취%고효액상색보법%이분미류제초제%농약잔류분석%수양
Cloud point extraction%High performance liquid chromatography%Biphenyl etherherbicides%Multi-residues analysis%Water
目的 建立同时测定水中多种二苯醚类除草剂残留的浊点萃取-高效液相色谱分析方法.方法 水样中8种二苯醚类除草剂(苯达松、氟磺胺草醚、三氟羧草醚、苯草醚、甲羧除草醚、乙羧氟草醚、除草醚、乙氧氟草醚)的残留经Triton X-114萃取,采用高效液相色谱法,用C_(18)色谱柱分离,以甲醇-三乙胺-盐酸溶液作流动相,梯度洗脱,在波长为300 nm处测定.采用Triton X-114进行浊点萃取,分别优化了影响萃取效率的表面活性剂浓度、水样pH值、盐浓度、平衡温度及时间等条件,并对待测物检测波长、流动相梯度洗脱、流动相pH值、流速和柱温等色谱条件进行了优化.结果 在优化的条件下,待测除草剂的质量浓度在0.05～2.00 mg/L范围内与其峰面积呈良好的线性关系(r=0.9991～0.9998),水样的平均加标回收率,除苯达松较低以外,均在80.1%～100.9%之间,相对标准偏差(RSD)为2.70 OA～6.40%;对于50.0 mL水样,本方法 的检出限为0.10～0.50 μg/L.结论 本法简便、快速、准确、灵敏度高,能满足环境水样中多种二苯醚类除草剂残留分析要求.
目的 建立同時測定水中多種二苯醚類除草劑殘留的濁點萃取-高效液相色譜分析方法.方法 水樣中8種二苯醚類除草劑(苯達鬆、氟磺胺草醚、三氟羧草醚、苯草醚、甲羧除草醚、乙羧氟草醚、除草醚、乙氧氟草醚)的殘留經Triton X-114萃取,採用高效液相色譜法,用C_(18)色譜柱分離,以甲醇-三乙胺-鹽痠溶液作流動相,梯度洗脫,在波長為300 nm處測定.採用Triton X-114進行濁點萃取,分彆優化瞭影響萃取效率的錶麵活性劑濃度、水樣pH值、鹽濃度、平衡溫度及時間等條件,併對待測物檢測波長、流動相梯度洗脫、流動相pH值、流速和柱溫等色譜條件進行瞭優化.結果 在優化的條件下,待測除草劑的質量濃度在0.05～2.00 mg/L範圍內與其峰麵積呈良好的線性關繫(r=0.9991～0.9998),水樣的平均加標迴收率,除苯達鬆較低以外,均在80.1%～100.9%之間,相對標準偏差(RSD)為2.70 OA～6.40%;對于50.0 mL水樣,本方法 的檢齣限為0.10～0.50 μg/L.結論 本法簡便、快速、準確、靈敏度高,能滿足環境水樣中多種二苯醚類除草劑殘留分析要求.
목적 건립동시측정수중다충이분미류제초제잔류적탁점췌취-고효액상색보분석방법.방법 수양중8충이분미류제초제(분체송、불광알초미、삼불최초미、분초미、갑최제초미、을최불초미、제초미、을양불초미)적잔류경Triton X-114췌취,채용고효액상색보법,용C_(18)색보주분리,이갑순-삼을알-염산용액작류동상,제도세탈,재파장위300 nm처측정.채용Triton X-114진행탁점췌취,분별우화료영향췌취효솔적표면활성제농도、수양pH치、염농도、평형온도급시간등조건,병대대측물검측파장、류동상제도세탈、류동상pH치、류속화주온등색보조건진행료우화.결과 재우화적조건하,대측제초제적질량농도재0.05～2.00 mg/L범위내여기봉면적정량호적선성관계(r=0.9991～0.9998),수양적평균가표회수솔,제분체송교저이외,균재80.1%～100.9%지간,상대표준편차(RSD)위2.70 OA～6.40%;대우50.0 mL수양,본방법 적검출한위0.10～0.50 μg/L.결론 본법간편、쾌속、준학、령민도고,능만족배경수양중다충이분미류제초제잔류분석요구.
Objective To determine residues of multiple biphenyl ether herbicides simultaneously in water using high performance liquid chromatography(HPLC)with cloud-point extraction.Methods The residues of eight biphenyl ether herbicides(including bentazone,fomesafen.acifluorfen,aclonifen,bifenox.fluoroglycofenethy,nitrofen,oxyfluorfen)in water samples were extracted with cloud-point extraction of Triton X-114.The analytes were separated and determined using reverse phase HPLC with ultraviolet detector at 300 nm.Optimized conditions for the pretreatment of water samples and the parameters of chromatographic separation applied.Results There was a good linear correlation between the concentration and the peak area of the analytes in the range of 0.05-2.00 mg/L(r=0.9991-0.9998).Except bentazone,the spiked recoveries of the biphenyl ether herbicides in the water samples ranged from 80.1%to 100.9%,with relative standard deviations ranging from 2.70%to 6.40%.The detection limit of the method ranged from 0.10 μg/L to 0.50 μg/L.Conclusion The proposed method is simple,rapid and sensitive,and can meet the requirements of determination of multiple biphenyl ether herbicides simultaneously in natural waters.
