CAJ | 학술논문

改进了淡水水体和沉积物中4种硝基呋喃代谢物呋喃唑酮代谢物（AOZ）、呋喃它酮代谢物（AMOZ）、呋喃妥因代谢物（AHD）、呋喃西林代谢物（SEM）的高效液相色谱串联质谱（LC －MS／MS）检测方法。方法采用内标法定量，提高了定量的准确性。水及沉积物样品直接进行衍生化后乙酸乙酯提取，化合物采用Thermo C18（5．0μm ，100 mm ×2．1 mm）色谱柱进行分离，以0．1％甲酸／甲醇－5 mmol／L乙酸铵水溶液（含0．1％甲酸）为流动相梯度洗脱。方法的线性范围为0．1～200 ng／m L ，r2≥0．999。空白水体在0．02、1．0、10.0 ng／L 3个加标水平下的平均回收率为75．4％～82．7％，相对标准偏差（RSD ）为3．2％～8．7％，检出限（LOD）和定量下限（LOQ）分别为0．01 ng／mL和0．02 ng／mL。沉积物样品在0．3、1．0、10μg／kg 3个加标水平下，平均回收率为77．9％～93．6％，RSD为2．5％～7．8％，检出限（LOD ）和定量下限（LOQ ）分别为0．1μg／kg和0．3μg ／kg。该方法灵敏度高、选择性好，适用于实际淡水养殖环境水体和底泥中4种硝基呋喃代谢物呋喃唑酮代谢物的残留测定。
개진료담수수체화침적물중4충초기부남대사물부남서동대사물（AOZ）、부남타동대사물（AMOZ）、부남타인대사물（AHD）、부남서림대사물（SEM）적고효액상색보천련질보（LC －MS／MS）검측방법。방법채용내표법정량，제고료정량적준학성。수급침적물양품직접진행연생화후을산을지제취，화합물채용Thermo C18（5．0μm ，100 mm ×2．1 mm）색보주진행분리，이0．1％갑산／갑순－5 mmol／L을산안수용액（함0．1％갑산）위류동상제도세탈。방법적선성범위위0．1～200 ng／m L ，r2≥0．999。공백수체재0．02、1．0、10.0 ng／L 3개가표수평하적평균회수솔위75．4％～82．7％，상대표준편차（RSD ）위3．2％～8．7％，검출한（LOD）화정량하한（LOQ）분별위0．01 ng／mL화0．02 ng／mL。침적물양품재0．3、1．0、10μg／kg 3개가표수평하，평균회수솔위77．9％～93．6％，RSD위2．5％～7．8％，검출한（LOD ）화정량하한（LOQ ）분별위0．1μg／kg화0．3μg ／kg。해방법령민도고、선택성호，괄용우실제담수양식배경수체화저니중4충초기부남대사물부남서동대사물적잔류측정。
A quantitative and qualitative method of high performance liquid chromatography tandem mass spectrometry (LC-MS/MS)was deveLoped for the analysis of 4 kinds of nitrofuran metabolites furazolidone metabolites (AOZ) ,furan it ketone metabolites (AMOZ) ,with nitrofurantoin metabo‐lites (AHD) ,nitrofural metabolites (SEM ) ,in water and sediment sample .Methods used internal standard determination ,then improveing the accuracy of the quantitative .Water and sediment samples directly was extracted using ethyl acetate after derivatization .The target compound separation was performed on a Thermo C18 (5 .0 μm ,100 mm × 2 .1 mm) with Methanol(containing 0 .1% formic acid) and 5 mmoL/L ammonium (containing 0 .1% formic acid) as mobile phase . The calibration curves of four analytes were linear in the range of 0 .1-100 ng/mL with correlation coefficients more than 0 .999 .The average recoveries of 4 kinds nitrofuran metabolites in blank water samples at three spiked concentration levels of 0 .02 ,1 .0 ,10 .0 ng/L were in the range of 75 .4% ~82 .7% with RSD of 3 .2% ~8 .7% ,and its limit of detection (LOD) and limit of quantitation (LOQ) were 0 .01 ng/mL and 0 .02ng/mL ,respectively .The average recoveries of 4 kinds nitrofuran metabolites in sediment at three spiked levels of 0 .3 ,1 .0 and 10 .0 μg/kg were ranged from 77 .9% to 93 .6% with RSDs of 2.5% ~7 .8% ,and its limit of detection(LOD) and limit of quantitation(LOQ) were 0 .1and 0 .3μg/kg ,The developed method was suitable for determining 4 kinds of nitrofuran metabolites in aquatic environmental water and sediment with high sensitivity and selectivity .