作　　者： ; ; ; ; (丁紫荣）;

机构地区： 湖南师范大学资源与环境科学学院

出　　处： 《环境工程学报》 2015年第5期2291-2296,共6页

摘　　要： 采用高效液相色谱-串联质谱(HPLC-MS/MS)检测,建立了地表水中13种药物及个人护理品的测定方法。水样用盐酸与氢氧化钠溶液调p H值至7.0左右,过固相萃取小柱进行富集,用14 m L甲醇洗脱。以C18柱为分离柱,0.01%甲酸的甲醇-0.01%甲酸水溶液为流动相,目标物在10 min内分离,在0.50~250μg/L范围内,13种化合物峰面积与内标物质峰面积之比与质量浓度的线性关系良好(>0.99),检出限在0.05~0.5 ng/L范围内。基质加标实验结果表明,13种化合物在水中的回收率分别在56.2%~123.2%之间(加标水平5 ng/m L)和58.0%~107.8%(加标水平50 ng/m L),相对标准偏差在1.60%~19.9%(n=6)之间。应用该方法测定了从2条纳污河流采集的10份水样,结果表明,除美托诺尔和普洛萘尔未被检出外,其余11药物的检出频率在30%~100%之间。在13种目标物质中,咖啡因的检测浓度最高达287.5ng/L,舒必利次之,为277.5 ng/L。本方法快速、准确,适用于地表水中PPCPs类的快速测定。 An analytical method was developed and validated for the determination of 13 pharmaceuticals and personal care products( PPCPs) using high performance liquid chromatography-tandem mass spectrometry.Water samples were concentrated by solid-phase extraction,and all the target PPCPs were efficiently extracted at p H 7. 0. The extracted PPCPs were eluted by 14 m L methanol. Separation was performed on a reverse-phase Cl8 column with gradient elution using a mixed solution composed of methanol( contain 0. 01% formic acid) and deionized( contain 0. 01% formic acid). The linear of alibration curve ranged from 0. 05 ~ 10. 00 mg / L and R2>0. 999. The limit of quantification( LOQ) ranged from 0. 05 ~ 0. 5 ng / m L. The results of recovery experiments showed that the average recoveries of the target compounds ranged from 53. 9% ~ 112% in the pure water samples spiked at 5 ng / m L,and ranged from 58. 0% ~ 107. 8% spiked at 50 ng / m L with the relative standard deviations ranged from 1. 6% ~ 19. 9%( n = 6). Ten surface water samples collected from two rivers in Guangzhou were detected. The results showed that metoprolol and propranolol were not detected,and the detection rates of the other eleven targets ranged from 30% to 100%. In the thirteen targets,the highest concentration of PPCPs was found to be caffeine( CF,287. 5 ng / L),with the following of sulpiride( SP,277. 5 ng / L). It proved that this analytical method is rapid,accurate and suitable for determination of PPCPs in surface water.

关 键 词： 固相萃取 药物及个人护理用品 高效液相色谱 串联质谱 地表水

领　　域： [环境科学与工程]