超高效液相色谱-三重四极杆质谱快速测定地表水中甲萘威、微囊藻毒素-LR、溴氰菊酯

Rapid Determination of Carbaryl,Microcystin-LR and Deltamethrin in Surface Water by Ultra-high Performance Liquid Chromatography-Triple QuadrupoleMass Spectrometry

基于超高效液相色谱-三重四极杆串联质谱技术(UPLC-MS/MS),建立了一种经简单过滤即可直接进样测定地表水中甲萘威、微囊藻毒素-LR、溴氰菊酯的分析方法。水样过0.22μm微孔滤膜后,经C18色谱柱(1.8μm,2.1 mm×50 mm),柱温40℃,流速0.3 mL/min,以甲醇和2 mmol/L乙酸铵水溶液(含0.1%甲酸)为流动相进行梯度洗脱;采用电喷雾正离子电离(ESI+),多反应监测模式(MRM)检测,外标法定量分析目标物。方法学验证结果表明3种目标物浓度在0.20~50.0μg/L范围线性关系良好,相关系数(R^(2))>0.9990,方法检出限为0.03~0.08μg/L,目标物平均加标回收率为89.3%~116%,相对标准偏差(RSD)为0.5%~9.6%(n=6)。所建立方法简便快捷、灵敏准确,适用于地表水中3种有机污染物同时快速测定。

Present work developed a direct injection method to detect carbaryl,microcystin-LR and deltamethrin in surface water based on ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS),which just required a simple filtration pretreatment before the determination.After being filtered by 0.22μm of microfiltration membrane,the water samples were gradient-eluted by methanol and 2 mmol/L ammonium acetate aqueous solution(containing 0.1%formic acid)under a flow rate of 0.3mL/min during passing through the eclipse plus C18 chromatographic column(1.8μm,2.1 mm×50 mm)with a column temperature of 40℃.The signals were thereby analyzed by a positive electrospray ionization(ESI+)using multiple reaction monitoring mode(MRM),which was further quantified by an external standard method.The methodological validation results demonstrated that:the developed method could lead to a good linearity relationship of these three organic pollutants in the range of 0.20-50.0μg/L;the correlation coefficients were higher than 0.9990(R^(2)>0.9990);the detection limit were 0.03-0.08μg/L;the average recoveries were 89.3%-116%;and the RSD ranged from 0.5%to 9.6%(n=6).Generally,present work developed a simple,rapid,sensitive and accurate method for the simultaneous detection of the above three organic pollutants in the surface water.