水中杀虫剂鱼藤酮的测定方法研究
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摘要
目的建立一种水中杀虫剂鱼藤酮的快速筛查方法,即利用超高效液相色谱-质谱(UPLC-MS)检测水样中鱼藤酮的方法。方法收集受污染的水样,用三氯甲烷振荡提取10 min,静置分层,取1 ml下层提取液经氮吹浓缩至近干后用1 ml乙腈溶解,溶解液过0.25μm滤膜后利用超高效液相色谱-质谱仪分离定性,外标法定量。结果在浓度为0.05μg/L～0.50μg/L时线性关系良好,线性方程为y=288 692x+641.932,线性相关系数(r)为0.999 2,方法的检出限以3倍标准差计算为0.60 ng/L,定量限以10倍标准差为2.0 ng/L。在低、中、高3种加标浓度水平下的回收率为63.8%～82.2%,相对标准偏差为3.01%～5.04%。结论本方法前处理操作简单快速,定性准确,检出限低,回收率高,精密度和准确度高。实际样品检测结果显示,本方法可以满足水样中鱼藤酮的快速筛查的要求。
Objective To establish a method for the determination of pesticides rotenone in water samples by ultra high performance liquid chromatography-mass spectrometry(UPLC-MS). Methods The contaminated water was collected, and extracted by trichloromethane for 10 min, then stayed for layering, the lower chloroform extract was taken to pass a 0.25 um filtration membrane for qualification by UPLC-MS, and external standard method was adopted for quantification. Results Good linearity was obtained within 0.05 μg/L-0.50 μg/L, with linear equation y=288 692x+641.932 and with correlation coefficient(r) of 0.999 2. The minimum detectable concentration was 0.60 ng/L based on 3 times of the SD, The quantitative limit was 2.0 ng/L based on 10 times of the SD. The recoveries at the three levels of low, medium and high spiked concentrations were within 63.8%-82.2%, and the relative standard deviations were within 3.01%-5.04%. Conclusion The method is simple, accurate and high sensitive. The actual sample testing results showed that this method can meet the requirements in rapid screening pesticides rotenone.
Objective To establish a method for the determination of pesticides rotenone in water samples by ultra high performance liquid chromatography-mass spectrometry(UPLC-MS). Methods The contaminated water was collected, and extracted by trichloromethane for 10 min, then stayed for layering, the lower chloroform extract was taken to pass a 0.25 um filtration membrane for qualification by UPLC-MS, and external standard method was adopted for quantification. Results Good linearity was obtained within 0.05 μg/L-0.50 μg/L, with linear equation y=288 692x+641.932 and with correlation coefficient(r) of 0.999 2. The minimum detectable concentration was 0.60 ng/L based on 3 times of the SD, The quantitative limit was 2.0 ng/L based on 10 times of the SD. The recoveries at the three levels of low, medium and high spiked concentrations were within 63.8%-82.2%, and the relative standard deviations were within 3.01%-5.04%. Conclusion The method is simple, accurate and high sensitive. The actual sample testing results showed that this method can meet the requirements in rapid screening pesticides rotenone.
引文
[1] Ferrante RJ, Schulz JB, Kowall NW, et al. Systemic administration of rotenone produces selective damage in the striarum and globus pallidus,but not in the substantia nigra[J]. Brain Res, 1997, 753(1): 157-162.
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[3] 张秋霜,陈颖,陈乃宏,等.鱼藤酮诱导大鼠帕金森样损伤及其机制研究[J].中国药物警戒.2017.14(9):513-517.
[4] 董兆君. 鱼腾酮的多巴胺神经元毒性与帕金森病[J].国外医学神经病学神经外科学分册,2001,28(5):357-360.
[5] 张晓艺,张秀尧,蔡欣欣,等.二维超高效液相色谱-三重四极杆-复合线性离子阱质谱联用快速测定全血和尿液中鱼藤酮[J].色谱,2017,35(5):482-486.
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[7] 潘峰,孙玮,张晓庆,等.高效液相色谱检测大鼠血浆鱼藤酮的含量[J].解放军预防医学杂志,2008,26(3):190-191.
[8] 胡道德,顾磊,刘皋林.反相高效液相色谱法测定毛鱼腾中鱼藤酮的含量[J].药学实践杂志,2007.25(3):159-161.
[9] 刘一平,王胜翔,宋稳成,等. QuEChERS-高效液相色谱-串联质谱法分析甘蓝和土壤中的鱼藤酮.农药科学与管理,2013,34(8):28-31.
[10] 杨方,郑丹萍,刘正才,等.液相色谱-串联质谱法同时检测水产品中苦参碱和鱼腾酮残留[J].分析化学研究简报,2011,39(4):556-559.
[11] 刘丽芬,吴永凤.2.5%复配农药吡虫啉·鱼藤酮乳油含量的高效液相色谱法测定[J].广州化工,2002,30(1):22-23.
[12] 刘哲鹏,倪德浩,陆丽芳.4.8%鱼藤酮·辣椒碱悬浮剂的高效液相色谱分析[J].农药,2009,48(6):424-426.
[13] 纪伟,崔玉兰,陈仁娟,等.高效逆流色谱法分离制备鱼腾根中的2种鱼腾酮类化合物[J].色谱, 2010,28(8):813-816.
[14] 李亚南,葛晓群.鱼藤酮毒性及含量测定方法研究进展[J]. 国际药学研究,2009,36(5):366-369.
[15] 武永昆,林军,叶敏,等.鱼藤酮的高效液相色谱分析方法研究[J].云南化工,2006,33(2):59-60.
[2] 邝贺龄.内科急症治疗学[M].第3版.上海科技出版社,1998:437.
[3] 张秋霜,陈颖,陈乃宏,等.鱼藤酮诱导大鼠帕金森样损伤及其机制研究[J].中国药物警戒.2017.14(9):513-517.
[4] 董兆君. 鱼腾酮的多巴胺神经元毒性与帕金森病[J].国外医学神经病学神经外科学分册,2001,28(5):357-360.
[5] 张晓艺,张秀尧,蔡欣欣,等.二维超高效液相色谱-三重四极杆-复合线性离子阱质谱联用快速测定全血和尿液中鱼藤酮[J].色谱,2017,35(5):482-486.
[6] 芦浩.气相色谱法分析鱼藤酮制剂的研究[J].农药,2004,43(2):83-85.
[7] 潘峰,孙玮,张晓庆,等.高效液相色谱检测大鼠血浆鱼藤酮的含量[J].解放军预防医学杂志,2008,26(3):190-191.
[8] 胡道德,顾磊,刘皋林.反相高效液相色谱法测定毛鱼腾中鱼藤酮的含量[J].药学实践杂志,2007.25(3):159-161.
[9] 刘一平,王胜翔,宋稳成,等. QuEChERS-高效液相色谱-串联质谱法分析甘蓝和土壤中的鱼藤酮.农药科学与管理,2013,34(8):28-31.
[10] 杨方,郑丹萍,刘正才,等.液相色谱-串联质谱法同时检测水产品中苦参碱和鱼腾酮残留[J].分析化学研究简报,2011,39(4):556-559.
[11] 刘丽芬,吴永凤.2.5%复配农药吡虫啉·鱼藤酮乳油含量的高效液相色谱法测定[J].广州化工,2002,30(1):22-23.
[12] 刘哲鹏,倪德浩,陆丽芳.4.8%鱼藤酮·辣椒碱悬浮剂的高效液相色谱分析[J].农药,2009,48(6):424-426.
[13] 纪伟,崔玉兰,陈仁娟,等.高效逆流色谱法分离制备鱼腾根中的2种鱼腾酮类化合物[J].色谱, 2010,28(8):813-816.
[14] 李亚南,葛晓群.鱼藤酮毒性及含量测定方法研究进展[J]. 国际药学研究,2009,36(5):366-369.
[15] 武永昆,林军,叶敏,等.鱼藤酮的高效液相色谱分析方法研究[J].云南化工,2006,33(2):59-60.
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