Rapid determination of four herbicides in urine with ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry
LI Qi1, LIU Huihui2, JI Lü1, XU Junqing1
1. Department of Laboratory, Lishui Center for Disease Prevention and Control, Lishui, Zhejiang 323000, China; 2. The Second People's Hospital of Lishui, Lishui, Zhejiang 323000, China
Abstract：Objective To establish a ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry method for rapid simultaneous determination of quinclorac, acetochlor, butachlor and metolachlor in urine. Methods Urine samples were diluted 10 times, prepared into the mixed standard solution, and subjected to gradient elution on the ACQUITY UPLC BEH C18 column (100 mm×2.1 mm, 1.7 μm) with 0.1% formic acid and acetonitrile as the mobile phase. The quinclorac, acetochlor, metolachlor and butachlor levels were determined using electrospray ionization-positive ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry with the multiple reaction monitoring mode. Results Four herbicides were effectively separated on the ACQUITY UPLC BEH C18 column (100 mm× 2.1 mm, 1.7 μm), and good linear relationships were observed for quinclorac, acetochlor and butachlor at 1 to 25 μg/L and for metolachlor at 0.2 to 25 μg/L, with all linear correlation coefficients of >0.999. The detection limts of quinclorac, acetochlor, butachlor and metolachlor were 0.10, 0.10, 0.20 and 0.01 μg/L, respectively. The recovery rates of quinclorac, acetochlor and butachlor were 107.42%, 93.94% and 90.27% from urine samples at a spiked level of 5 µg/L, with relative standard deviations of 4.82%, 3.84% and 6.76%, and the recovery rate of metolachlor was 89.51% at a spiked level of 0.5 µg/L, with a relative standard deviation of 8.98%. Conclusion The chromatography and mass spectrometry conditions are optimized in this ultra-high performance liquid chromatography-tandem mass spectrometry, which is effective for rapid simultaneous determination of quinclorac, acetochlor, metolachlor and butachlor in urine samples.
李启, 刘慧慧, 纪律, 徐峻卿. 超高效液相色谱-串联三重四级杆质谱法快速测定尿液中4种除草剂[J]. 预防医学, 2023, 35(2): 176-179.
LI Qi, LIU Huihui, JI Lü, XU Junqing. Rapid determination of four herbicides in urine with ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry. Preventive Medicine, 2023, 35(2): 176-179.
