Determination of Glufosinate, Glyphosate and Aminomethylphosphonic Acid in Water by High Performance Liquid Chromatography with Ultrasound Assisted Derivatization
摘 要
取2 mL水样,依次加入6 mg二水合柠檬酸三钠、1 mL 0.05 mol·L-1四硼酸钠溶液和2 mL 1 g·L-1 9-芴甲基氯甲酸酯(FMOC-Cl)溶液,在常温、250 W超声功率下衍生10 min。加入0.40 g氯化钠进行盐析,涡旋2 min,静置1 min,收集下层水相过0.45 μm滤膜,滤液用高效液相色谱法分析。以PAH C18色谱柱作固定相,不同体积比乙腈和0.2%(体积分数)磷酸溶液的混合溶液作流动相进行梯度洗脱分离,荧光检测器检测。结果显示:草铵膦、草甘膦、氨甲基膦酸的质量浓度均在0.400~50.0 μg·L-1内和其对应的衍生产物的峰面积呈线性关系,检出限(3.143s)分别为0.2,0.1,0.1 μg·L-1。按照标准加入法进行回收试验,回收率为87.6%~100%,测定值的相对标准偏差(n=6)为5.7%~12%。方法用于实际水样的分析,检出结果均为阴性。
Abstract
The 2 mL of water sample was taken, and 6 mg of trisodium citrate dihydrate, and 1 mL of 0.05 mol·L-1 sodium tetraborate solution, and 2 mL of 1 g·L-1 9-fluorene methyl chloroform (FMOC-Cl) solution were added sequentially. The mixed solution was reacted to derivatize targets at room temperature with ultrasonic power of 250 W for 10 min. Then 0.40 g of sodium chloride was added for salting out, and the mixture was vortexed for 2 min, and settled for 1 min. The lower water phase was collected, and passed through a 0.45 μm filter membrane, and the filtrate was analyzed by high performance liquid chromatography. PAH C18 chromatographic column was used as the stationary phase, and the mixed solutions composed of acetonitrile and 0.2% (volume fraction) phosphoric acid solution at different volume ratios were used as the mobile phase for gradient elution separation, and fluorescence detector was used for detection. It was shown that linear relationships between values of the mass concentration of glufosinate, glyphosate, and aminomethylphosphonic acid and the peak area of their derivatization products were kept in the range of 0.400-50.0 μg·L-1, with detection limits (3.143s) of 0.2, 0.1, 0.1 μg·L-1, respectively. Test for recovery was made according to the standard addition method, giving recoveries in the range of 87.6%-100%, and RSDs (n=6) of the determined values ranged from 5.7% to 12%. The proposed method was used for the analysis of actual water samples, and the detection results were all negative.
中图分类号 O657.72 DOI 10.11973/lhjy-hx202311015
所属栏目 工作简报
基金项目 湖北省地质局科研项目(KJ2021-18、KJ2022-36)
收稿日期 2022/6/20
修改稿日期
网络出版日期
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联系人作者宋洲(sz001123@126.com)
备注罗火焰,工程师,主要从事环境检测研究工作
引用该论文: LUO Huoyan,SONG Zhou,JI Yiping,PI Shishi,ZHOU Yuqi,TAN Kai. Determination of Glufosinate, Glyphosate and Aminomethylphosphonic Acid in Water by High Performance Liquid Chromatography with Ultrasound Assisted Derivatization[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2023, 59(11): 1332~1336
罗火焰,宋洲,吉义平,皮施施,周宇齐,谭凯. 超声辅助衍生-高效液相色谱法测定水中草铵膦、草甘膦及氨甲基膦酸的含量[J]. 理化检验-化学分册, 2023, 59(11): 1332~1336
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参考文献
【1】简秋,胡德禹,张钰萍,等.草铵膦在土壤中的残留检测方法及消解动态[J].农药, 2015,54(3):201-203.
【2】孙文闪,诸骏杰,钟寒辉,等.固相萃取净化-超高效液相色谱-三重四极杆质谱法测定土壤中草铵膦、草甘膦及其代谢物氨甲基膦酸[J].理化检验-化学分册, 2021,57(4):322-326.
【3】周芹,吴玉梅.超高效液相色谱串联质谱非衍生化法测定土壤中草甘膦及其代谢物氨甲基膦酸含量[J].中国农学通报, 2020,36(27):72-80.
【4】何书海,曹小聪,吴海军,等.直接进样超高效液相色谱-三重四极杆质谱法快速测定环境水样中草甘膦、氨甲基膦酸、草铵膦及乙烯利残留[J].色谱, 2019,37(11):1179-1184.
【5】张燕,舒平,陆敏,等.分散固相萃取/衍生化-高效液相色谱-串联质谱法同时测定水和食品中草甘膦、草铵膦和氨甲基膦酸残留[J].食品安全质量检测学报, 2017,8(4):1422-1428.
【6】张文,闫君,陈婷,等.离子色谱法同时测定饮用水中强极性农药草甘膦、草铵膦、乙烯利和调节膦[J].分析试验室, 2021,40(3):307-311.
【7】董建芳,董会军,李义,等.柱前衍生-液相色谱-串联质谱法测定环境水体中草甘膦及其代谢产物的影响因素研究[J].河北工业科技, 2022,39(1):71-78.
【8】杨华梅,杭莉,刁春霞,等.超高效液相色谱-串联质谱法同时直接测定草甘膦和草铵膦及其代谢物[J].分析科学学报, 2020,36(4):606-610.
【9】陈磊,何香伟,李晓贝,等.HPLC-MS/MS检测黑木耳中草甘膦、草铵膦及代谢物残留[J].分析试验室, 2021,40(5):535-540.
【10】罗本越.QuEChERS-LC/MS/MS快速测定不同茶叶中草甘膦、氨甲基膦酸及草铵膦的残留[J].福建分析测试, 2022,31(3):14-20.
【11】刘文静,林晶,傅建炜,等.超高效液相-串联质谱法测定茶叶中草甘膦、草铵膦、氨甲基膦酸残留[J].中国农学通报, 2020,36(25):129-136.
【12】赵志东,孟娇,张显强,等.固相萃取-离子色谱法测定血液中草甘膦及其代谢物氨甲基膦酸[J].理化检验-化学分册, 2020,56(3):349-351.
【13】KOLLER V J, FVRHACKER M, NERSESYAN A, et al. Cytotoxic and DNA-damaging properties of glyphosate and Roundup in human-derived buccal epithelial cells[J]. Archives of Toxicology, 2012,86(5):805-813.
【14】MESNAGE R, BERNAY B, SÉRALINI G E. Ethoxylated adjuvants of glyphosate-based herbicides are active principles of human cell toxicity[J]. Toxicology, 2013,313(2/3):122-128.
【15】MAO Y C, HUNG D Z, WU M L, et al. Acute human glufosinate-containing herbicide poisoning[J]. Clinical Toxicology, 2012,50(5):396-402.
【16】CHIESA L M, NOBILE M, PANSERI S, et al. Detection of glyphosate and its metabolites in food of animal origin based on ion-chromatography-high resolution mass spectrometry (IC-HRMS)[J]. Food Additives & Contaminants:Part A, 2019,36(4):592-600.
【17】杨华梅,杭莉.柱前衍生-固相萃取-高效液相色谱法测定饮用水中草甘膦和氨甲基膦酸[J].理化检验-化学分册, 2015,51(4):474-477.
【18】张蓓蓓,张立志,章勇.水中草甘膦和氨甲基膦酸的柱前衍生-液相色谱方法研究[J].环境监控与预警, 2015,7(2):13-16.
【2】孙文闪,诸骏杰,钟寒辉,等.固相萃取净化-超高效液相色谱-三重四极杆质谱法测定土壤中草铵膦、草甘膦及其代谢物氨甲基膦酸[J].理化检验-化学分册, 2021,57(4):322-326.
【3】周芹,吴玉梅.超高效液相色谱串联质谱非衍生化法测定土壤中草甘膦及其代谢物氨甲基膦酸含量[J].中国农学通报, 2020,36(27):72-80.
【4】何书海,曹小聪,吴海军,等.直接进样超高效液相色谱-三重四极杆质谱法快速测定环境水样中草甘膦、氨甲基膦酸、草铵膦及乙烯利残留[J].色谱, 2019,37(11):1179-1184.
【5】张燕,舒平,陆敏,等.分散固相萃取/衍生化-高效液相色谱-串联质谱法同时测定水和食品中草甘膦、草铵膦和氨甲基膦酸残留[J].食品安全质量检测学报, 2017,8(4):1422-1428.
【6】张文,闫君,陈婷,等.离子色谱法同时测定饮用水中强极性农药草甘膦、草铵膦、乙烯利和调节膦[J].分析试验室, 2021,40(3):307-311.
【7】董建芳,董会军,李义,等.柱前衍生-液相色谱-串联质谱法测定环境水体中草甘膦及其代谢产物的影响因素研究[J].河北工业科技, 2022,39(1):71-78.
【8】杨华梅,杭莉,刁春霞,等.超高效液相色谱-串联质谱法同时直接测定草甘膦和草铵膦及其代谢物[J].分析科学学报, 2020,36(4):606-610.
【9】陈磊,何香伟,李晓贝,等.HPLC-MS/MS检测黑木耳中草甘膦、草铵膦及代谢物残留[J].分析试验室, 2021,40(5):535-540.
【10】罗本越.QuEChERS-LC/MS/MS快速测定不同茶叶中草甘膦、氨甲基膦酸及草铵膦的残留[J].福建分析测试, 2022,31(3):14-20.
【11】刘文静,林晶,傅建炜,等.超高效液相-串联质谱法测定茶叶中草甘膦、草铵膦、氨甲基膦酸残留[J].中国农学通报, 2020,36(25):129-136.
【12】赵志东,孟娇,张显强,等.固相萃取-离子色谱法测定血液中草甘膦及其代谢物氨甲基膦酸[J].理化检验-化学分册, 2020,56(3):349-351.
【13】KOLLER V J, FVRHACKER M, NERSESYAN A, et al. Cytotoxic and DNA-damaging properties of glyphosate and Roundup in human-derived buccal epithelial cells[J]. Archives of Toxicology, 2012,86(5):805-813.
【14】MESNAGE R, BERNAY B, SÉRALINI G E. Ethoxylated adjuvants of glyphosate-based herbicides are active principles of human cell toxicity[J]. Toxicology, 2013,313(2/3):122-128.
【15】MAO Y C, HUNG D Z, WU M L, et al. Acute human glufosinate-containing herbicide poisoning[J]. Clinical Toxicology, 2012,50(5):396-402.
【16】CHIESA L M, NOBILE M, PANSERI S, et al. Detection of glyphosate and its metabolites in food of animal origin based on ion-chromatography-high resolution mass spectrometry (IC-HRMS)[J]. Food Additives & Contaminants:Part A, 2019,36(4):592-600.
【17】杨华梅,杭莉.柱前衍生-固相萃取-高效液相色谱法测定饮用水中草甘膦和氨甲基膦酸[J].理化检验-化学分册, 2015,51(4):474-477.
【18】张蓓蓓,张立志,章勇.水中草甘膦和氨甲基膦酸的柱前衍生-液相色谱方法研究[J].环境监控与预警, 2015,7(2):13-16.
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