单一溶剂处理-气相色谱测定杭白菊中残留含磷有机农药
GC Determination of Residual Organophosphorus Pesticides in Hangzhou White Chrysanthemum by Treatment of Samples with Single Extractant
摘 要
单独用丙酮作为溶剂提取杭白菊样品中残留的含磷有机农药.所得提取液经CARB/NH2固相萃取柱净化后,在30 ℃旋转蒸发浓缩至1~2 mL,再用吹氮方法进一步浓缩至0.4 mL,最后将此丙酮溶液定容至0.5 mL,供气相色谱测定用.在DB-1701石英毛细管色谱柱上,8种农药达到很好分离并用氮磷检测器进行测定.测得8种农药的工作曲线线性范围均在0.05~5.0 mg·L-1以内,8种农药的检出限(3S/N)在0.009~0.028 μg·g-1之间.对方法的精密度和回收率作了试验,测得其相对标准偏差(n=6)在5.45%~7.27%之间,回收率在67.3%~104.0%之间.
含磷有机农药
固相萃取
丙酮
杭白菊
GC
Organophosphorus pesticides
Solid-phase extraction (SPE)
Acetone
Hangzhou white chrysanthemum
Abstract
Residual amounts of organophosphorus pesticides in samples of Hangzhou white chrysanthemum were extracted with acetone singly,and the extract obtained were purified by the CARB/NH2 SPE column. Eluate from the column was concentrated to 1-2 mL by rotary evaporation at 30 ℃ and then to ca. 0.4 mL by N2-blowing. After making up to 0.5 mL,the solution in acetone was used for GC determination. By using the DB-1701 quartz capillary chromatographic column,8 organophosphorus pesticides were separated and determined by NPD. Ranges of linearity of the working curves for these 8 pesticides were kept within 5.0 mg·L-1,and the values of detection limit (3S/N) found were in the range of 0.009-0.028 μg·g-1. Precision and recovery of the method were tested,and values of RSD′s (n=6) and of recovery found were in the ranges of 5.45%-7.27% and 67.3%-104.0% respectively.
中图分类号 O657.7
所属栏目 工作简报
基金项目 桐乡市第三批科技项目(200703096)
收稿日期 2008/4/11
修改稿日期
网络出版日期
作者单位点击查看
备注吴晶(1981-),女,浙江桐乡人,检验技师,硕士,从事食品理化检验工作.
引用该论文: WU Jing,CHEN Guo-zheng,QIAN Hong-zhi,WANG Xuan-zheng. GC Determination of Residual Organophosphorus Pesticides in Hangzhou White Chrysanthemum by Treatment of Samples with Single Extractant[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(7): 822～824
吴晶,陈国征,钱洪智,王炫征. 单一溶剂处理-气相色谱测定杭白菊中残留含磷有机农药[J]. 理化检验－化学分册, 2009, 45(7): 822～824
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【3】陈伟琪,侯小凤,张珞平.SPME,GC联用测定蔬菜中残留有机磷农药的方法研究[J].厦门大学学报:自然科学版,2000,39(4):509-515．
【4】胡飞凤,林晓.EDTA络合滴定法测定太子宝颗粒中葡萄糖酸钙的含量[J].海峡药学,2003,6(15):34-36．
【5】董顺福,朱志国,刘伟明,等.原子吸收分光光度法测定利心丸中钙、镁、铁、锰、铜、锌的含量[J].光谱学与光谱分析,2001,3(21):391-392．
【6】崔荣,徐汉卿,冯捷.马勃中微量元素的测定[J].微量元素与健康研究,2003,20(1):26-28．
【7】董顺福,朱志国,奚克生.治疗冠心病中成药物中氟钙铜的含量[J].第四军医大学学报,2002,23(11):26-27．
【8】张嫦,周小菊,刘东,等.药用碳酸锂中钠钾钙镁的测定方法研究[J].西南民族学院学报:自然科学版,2003,29(2):156-157．
【9】郑璐侠,段更利,高敏洁,等.反相高压液相色谱法测定亚叶酸钙制剂的含量及稳定性考察[J].中国新药与临床杂志,2003,22(2):74-75．
【10】潘教麦,李在均,张其颖,等.新显色剂及其在光度分析中的应用[M].北京:化学工业出版社,2003:73-74．
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