论文部分内容阅读
目的建立同时测定尿中9种单羟基多环芳烃(OH-PAHs,即1-羟基萘、2-羟基萘、3-羟基芴、3-羟基菲、1-羟基芘、3-羟基■、6-羟基■、3-羟基苯并蒽和9-羟基苯并芘)的固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)法。方法将10 ml尿样经酶水解、C18固相萃取柱(500 mg,3 ml)提取富集后,用Waters ACQUITY UPLC BEH C_(18)色谱柱(2.1×100 mm,1.7μm)分离,在三重四级杆串联质谱负离子模式下检测,以内标法定量分析。结果尿中9种目标化合物在0.102~40 ng/ml范围内均呈良好的线性关系(r>0.999),检出限(S/N=3)为0.01~0.32 ng/ml,样品在1.6、4.0、10 ng/ml浓度水平的平均加标回收率为91.5%~128%,相对标准偏差(RSD)<15%。结论该方法用时短,灵敏度高,准确度好,精密度高,适合人群尿中多环芳烃代谢物的监测。
OBJECTIVE To establish a method for the simultaneous determination of nine monohydroxy polycyclic aromatic hydrocarbons (OH-PAHs) in urine (ie, 1-hydroxynaphthalene, 2-hydroxynaphthalene, 3-hydroxyfluorene, -Hydroxy-, 3-hydroxybenzanthracene and 9-hydroxybenzopyrene) by SPE-UPLC-MS / MS. Methods After the 10 ml urine samples were extracted by C18 SPE (500 mg, 3 ml), they were separated by a Waters ACQUITY UPLC BEH C 18 column (2.1 × 100 mm, 1.7 μm) Triple quadrupole mass spectrometry negative ion mode detection, quantitative analysis by internal standard method. Results There were good linear relationships (r> 0.999) for the nine target compounds in urine from 0.102 to 40 ng / ml with a detection limit (S / N = 3) of 0.01 to 0.32 ng / The average spike recoveries of 4.0 and 10 ng / ml ranged from 91.5% to 128% with relative standard deviations (RSDs) <15%. Conclusion The method is short-time, high sensitivity, good accuracy, high precision, suitable for the monitoring of urinary PAH metabolites.