中华预防医学杂志
中華預防醫學雜誌
중화예방의학잡지
CHINESE JOURNAL OF
2013年
5期
459-462
,共4页
农药%固相萃取%水%高效液相色谱串联质谱法
農藥%固相萃取%水%高效液相色譜串聯質譜法
농약%고상췌취%수%고효액상색보천련질보법
Pesticides%Solid phase extraction%Water%High performance liquid chromatography-tandem mass spectrometry
目的 建立同时测定生活饮用水中灭草松、2,4-滴、呋喃丹、甲萘威、莠去津和五氯酚6种农药的液相色谱-串联质谱方法,为《生活饮用水标准检验方法》(GB/T 5750-2006)的修订提供参考,并对江苏境内12个集中式供水出厂水中上述6种农药含量进行评估.方法 用盐酸调节水样至pH≤2,取10 ml水样经反相固相萃取小柱富集,丙酮洗脱,氮吹仪浓缩,溶剂转换后,以甲醇和(或)水为流动相,经C18液相色谱柱分离,用液相色谱-串联质谱仪外标法测定,并对方法的检测限、准确度和精密度进行评价.检测了江苏境内12个集中式供水出厂水中上述6种农药含量.结果 采用本检测方法,6种农药最低检测质量浓度在0.02～0.41 μg/L之间,回收率在75％～115％之间,RSD在2％ ～ 10％之间.江苏境内12个集中式供水出厂水中上述6种农药含量均小于最低检测浓度.结论 建立的方法可同时检测6种农药,检测效率高,废液排放少,能更好地满足饮用水卫生监测的需要.
目的 建立同時測定生活飲用水中滅草鬆、2,4-滴、呋喃丹、甲萘威、莠去津和五氯酚6種農藥的液相色譜-串聯質譜方法,為《生活飲用水標準檢驗方法》(GB/T 5750-2006)的脩訂提供參攷,併對江囌境內12箇集中式供水齣廠水中上述6種農藥含量進行評估.方法 用鹽痠調節水樣至pH≤2,取10 ml水樣經反相固相萃取小柱富集,丙酮洗脫,氮吹儀濃縮,溶劑轉換後,以甲醇和(或)水為流動相,經C18液相色譜柱分離,用液相色譜-串聯質譜儀外標法測定,併對方法的檢測限、準確度和精密度進行評價.檢測瞭江囌境內12箇集中式供水齣廠水中上述6種農藥含量.結果 採用本檢測方法,6種農藥最低檢測質量濃度在0.02～0.41 μg/L之間,迴收率在75％～115％之間,RSD在2％ ～ 10％之間.江囌境內12箇集中式供水齣廠水中上述6種農藥含量均小于最低檢測濃度.結論 建立的方法可同時檢測6種農藥,檢測效率高,廢液排放少,能更好地滿足飲用水衛生鑑測的需要.
목적 건립동시측정생활음용수중멸초송、2,4-적、부남단、갑내위、유거진화오록분6충농약적액상색보-천련질보방법,위《생활음용수표준검험방법》(GB/T 5750-2006)적수정제공삼고,병대강소경내12개집중식공수출엄수중상술6충농약함량진행평고.방법 용염산조절수양지pH≤2,취10 ml수양경반상고상췌취소주부집,병동세탈,담취의농축,용제전환후,이갑순화(혹)수위류동상,경C18액상색보주분리,용액상색보-천련질보의외표법측정,병대방법적검측한、준학도화정밀도진행평개.검측료강소경내12개집중식공수출엄수중상술6충농약함량.결과 채용본검측방법,6충농약최저검측질량농도재0.02～0.41 μg/L지간,회수솔재75％～115％지간,RSD재2％ ～ 10％지간.강소경내12개집중식공수출엄수중상술6충농약함량균소우최저검측농도.결론 건립적방법가동시검측6충농약,검측효솔고,폐액배방소,능경호지만족음용수위생감측적수요.
Objective To develop an analytical method for simultaneous determination of 6 pesticides,namely bentazone,2,4-dichlorophenoxyacetic acid,carbofuran,carbaryl,atrazine and pentachlorophenol,in drinking water by high performance liquid chromatography-tandem mass spectrometry,and thereby to provide a reference to revise the Health Standards for Drinking Water (GB/T 5750-2006).Meanwhile,to evaluate the content of the above 6 pesticides in the drinking water samples supplied by 12 centralized water plants in Jiangsu province.Methods The 10 ml water sample was acidized by hydrochloric acid to pH ≤ 2,and then concentrated by solid phase extraction cartridge and eluted with acetone.The solvent was changed into methanol after drying by nitrogen blow.The target compounds were separated by C18 column using methanol/water as mobile phase,and detected by mass spectrometry with multi-reaction-monitoring(MRM) mode.The repeatability and sensitivity of the assay were evaluated.The drinking water samples from the 12 water plants were then detected.Results In this experimental method,the minimum detectable concentration were around 0.02-0.41 μg/L,with the recovery rate at 75％-115％,and the RSD between 2％ and 10％.Under the experimental condition,there were no pesticides detected in the drinking water samples from the 12 centralized water plants.Conclusion The method is efficient and environment-friendly,with little discharge of effluent,which could meet the requirement of the drinking water monitor.
