CAJ | 학술논문

建立了乳制品中三氯生、三氯卡班、双酚A和壬基酚4种内分泌干扰物的在线固相萃取超高压液相色谱-串联质谱(On-line SPE LC-MS/MS)检测方法。液态乳制品或奶粉样品中加入乙酸缓冲液,目标物经β-葡糖醛酸苷肽酶/芳基磺酸酯酶酶解后,用乙腈提取,冷冻离心10 min后,取上清液,用水稀释,在线固相萃取串联质谱法测定。样品溶液经Xbridge C8柱富集,BEH C18色谱柱分离,甲醇和水梯度洗脱,三重四极杆质谱电喷雾负离子模式下采集数据,同位素内标法定量。4种目标化合物的线性范围为0.005~5.0μg/L,相关系数R2>0.99；方法的定量限为0.03~1.0μg/kg,3个添加水平的平均加标回收率为80.2％~106.7％, RSD<15％。本方法快速、简单、灵敏度高,适用于乳制品中4种内分泌干扰物的同时检测。应用本方法对原料乳和北京市售液奶样品进行了分析,结果表明,壬基酚的检出率最高。
건립료유제품중삼록생、삼록잡반、쌍분A화임기분4충내분비간우물적재선고상췌취초고압액상색보-천련질보(On-line SPE LC-MS/MS)검측방법。액태유제품혹내분양품중가입을산완충액,목표물경β-포당철산감태매/방기광산지매매해후,용을정제취,냉동리심10 min후,취상청액,용수희석,재선고상췌취천련질보법측정。양품용액경Xbridge C8주부집,BEH C18색보주분리,갑순화수제도세탈,삼중사겁간질보전분무부리자모식하채집수거,동위소내표법정량。4충목표화합물적선성범위위0.005~5.0μg/L,상관계수R2>0.99；방법적정량한위0.03~1.0μg/kg,3개첨가수평적평균가표회수솔위80.2％~106.7％, RSD<15％。본방법쾌속、간단、령민도고,괄용우유제품중4충내분비간우물적동시검측。응용본방법대원료유화북경시수액내양품진행료분석,결과표명,임기분적검출솔최고。
A simple analytical method by means of on-line solid phase extraction followed liquid chromatography-tandem mass spectrometry ( SPE-LC-MS/MS) was developed for the simultaneous quantitation of 4 endocrine disruptors ( triclosan, triclocarban, bisphenol A and nonylphenol) in dairy products. Infant formula and milk samples were dissolved in acetic acid buffer and hydrolyzed by β-glucuronidase/arylsulfatase. Acetonitrile was used as the extract. Then, the mixture was freeze-centrifuged for 10 min and the supernatant was diluted with water, and analyzed via on-line SPE-LC-MS/MS. The sample extracts were concentrated by an Xbridge C8 cartridge and separated on a BEH C18 column with a gradient mobile phase of methanol and water; then analyzed by triple quadrupole mass spectrometry. Mass acquisition was conducted under negative electrospray ionization mode. Quantification was performed by isotopic internal standard calibration. Acceptable linearity (R2>0. 99) was achieved over the range of 0. 005-5. 0 μg/L, with limits of quantification of 0. 03-1. 0μg/kg. Average recoveries of four target compounds (spiked at three concentration levels) ranged from 80. 2%-106. 7%,with relative standard deviation less than 15%. Due to its rapidity, simplicity, and high sensitivity, the method is suitable for the analysis of endocrine disruptors in dairy products. It has been applied in the analysis of raw milk and milk products collected in Beijing. As a result, nonylphenol was found with a high detectable frequency.