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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
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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 |
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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.
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Received: 08 September 2022
Revised: 17 January 2022
Published: 21 February 2023
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[1] GROSSMANN K,KWIATKOWSKI J.The mechanism of quinclorac selectivity in grasses[J].Pestic Biochem Physiol,1995(51):150-161. [2] COLAZZO M,PARJA L,CESIO M V,et al.Multi-residue method for trace pesticide analysis in soils by LC-QQQ-MS/MS and its application to real samples[J].Int J Environ Anal Chem,2018,98(14):1292-1308. [3] 纪律,李启,李伟营,等.超高效液相色谱-三重四级杆质谱法测定水中二氯喹啉酸残留[J].预防医学,2020,32(12):1283-1286. [4] 常青云,周欣,高书涛,等.悬浮固化液相微萃取-气相色谱联用测定水样中酰胺类除草剂残留[J].分析化学,2012,40(4):523-528. [5] 钱训,谭小会.液相色谱法同时测定除草剂中乙草胺、异噁草酮和2,4-滴丁酯的含量[J].食品安全质量检测学报,2018,17(9):4546-4549. [6] 李建中,储晓刚,蔡会霞,等.高效液相色谱法同时测定大豆中12种酰胺类除草剂的残留量[J].色谱,2006,24(6):585-588. [7] 王晓燕,季仁东,陈仁文.异丙甲草胺农药残留吸收光谱检测方法研究[J].光谱学与光谱分析,2019,39(1):180-184. [8] 李菊颖,郭欣妍,何健,等.玉米粉中吡虫啉、三唑酮、乙草胺与异丙甲草胺的QuEChERS/高效液相色谱-串联质谱快速检测[J].分析测试学报,2017,36(6):783-787. [9] 梅文泉,黎其万,方海仙,等.QuEChERS-气相色谱-质谱法测定土壤中6种酰胺类除草剂残留[J].色谱,2017,35(12):1317-1321. [10] 李启,纪律,徐峻卿,等.超高效液相色谱-串联质谱法快速测定血浆中乙草胺和异丙甲草胺[J].中国卫生检验杂志,2022,32(7):798-801. [11] 马力,金永堂.湖州市农药中毒病例特征分析[J].预防医学,2020,32(3):301-303,306. |
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