HPLC-MS/MS Determination of Simazine in Urine with Solid Phase Extraction
摘 要
尿液样品经Waters Oasis HLB LP柱萃取,乙腈洗脱,采用高效液相色谱-串联质谱法测定洗脱液中西玛津的含量。以Eclipse Plus C18色谱柱为固定相,以70%(体积分数)乙腈溶液为流动相,串联质谱分析中采用电喷雾离子源正离子模式和多反应监测模式。西玛津的质量浓度在500.0 μg·L-1以内与其对应的峰面积呈线性关系,检出限(3s/k)为0.91 μg·L-1,测定下限(10s/k)为3.03 μg·L-1。以空白样品为基体进行加标回收试验,所得回收率为80.7%~84.0%,测定值的日内相对标准偏差(n=6)和日间相对标准偏差(n=4)分别为1.8%~2.9%,6.8%~9.1%。
Abstract
The urine sample was extracted with Waters Oasis HLB LP column, and the column was eluted by acetonitrile. HPLC-MS/MS was applied to the determination of simazine in the eluate. Eclipse Plus C18 chromatographic column was used as stationary phase, and 70% (volume fraction) acetonitrile solution was used as mobile phase. ESI+ and multi-reactions monitor mode were adopted in MS/MS. Linear relationship between values of peak area and mass concentration of simazine was kept in the range within 500.0 μg·L-1, with detection limit (3s/k) of 0.91 μg·L-1 and lower limit of determination (10s/k) of 3.03 μg·L-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 80.7%-84.0%, with intra-day RSDs (n=6) and inter-day RSDs (n=4) of determined values in the ranges of 1.8%-2.9% and 6.8%-9.1%, respectively.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202012005
所属栏目 工作简报
基金项目 江南大学公共卫生研究中心青年项目(JUPH201843)
收稿日期 2019/12/26
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联系人作者常薇(805958905@qq.com)
备注王晓嫚,硕士研究生,研究方向为卫生检验与检疫
引用该论文: WANG Xiaoman,CHANG Wei,WU Yukang,QIU Dechao,MEI Yong. HPLC-MS/MS Determination of Simazine in Urine with Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(12): 1272~1276
王晓嫚,常薇,吴宇伉,邱德超,梅勇. 固相萃取-高效液相色谱-串联质谱法测定尿液中西玛津[J]. 理化检验-化学分册, 2020, 56(12): 1272~1276
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【5】QU S U, LIU B, HONG J, et al. Determination of eleven triazine pesticides in soil samples by accelerated solvent extraction-high performance liquid chromatography[J]. Environmental Chemistry, 2017,36(3):628-634.
【6】王晓春,王广,焦杏春.三嗪类除草剂分析方法研究进展[J].农药, 2011,50(5):320-324.
【7】汪力.水中农药类典型内分泌干扰物的去除特性及机理研究[D].上海:同济大学, 2006.
【8】宋国春,李瑞娟,刘同金,等.西玛津在茶叶及土壤中的残留与安全性评价[J].贵州农业科学, 2017,45(1):55-58.
【9】姜莉,于凤芹,于会文.出口肉和肉制品中西玛津残留量的快速测定[J].现代科学仪器, 2000,22(1):30-31.
【10】任兵.西玛津降解菌的降解特性及代谢途径研究[D].大庆:黑龙江八一农垦大学, 2016.
【11】王兴琴,潘锦勇.西玛津在玉米植株中的残留消解动态研究[J].安徽农学通报, 2010,16(17):39-41.
【12】罗方方,王艳君,叶玫,等.气相色谱-质谱法测定渔业水质中8种除草剂的残留量[J].渔业科学进展, 2015,36(4):132-138.
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【14】LI Y N, WU H L, QING X D, et al. Quantitative analysis of triazine herbicides in environmental samples by using high performance liquid chromatography and diode array detection combined with second-order calibration based on an alternating penalty trilinear decomposition algorithm[J]. Analytica Chimica Acta, 2010,678(1):26-33.
【15】DE OLIVEIRA SILVA R, DE CASTRO R C, MILHOME M A L, et al. Liquid chromatography-electrospray ionization-tandem mass spectrometry method for determination of twenty multi-class pesticide residues in cashew[J]. LWT-Food Science and Technology, 2014,59(1):21-25.
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