【求助】土壤中吡虫啉的分析方法

楼主，关于吡虫啉的分析方法，在论坛中已有讨论见链接:
http://www.instrument.com.cn/bbs/shtml/20070901/965432/
此外，有篇文章你可以参考：

楼主参考一下这个标准。http://www.instrument.com.cn/show/download/shtml/062332.shtml

谢谢，这个方法我有。不过，我还是想找一下土壤中的方法

不一定非要找到确定的方法才能做，可以参考现有方法，结合自己的样品对方法进行改进。

应助达人

土壤的前处理不是很复杂,和蔬菜上的差不多.

Development and Validation of Analytical Method for Determination of Imidacloprid Residues in/on Soil and Water by HPLC
Abstract
A rapid, sensitive and reliable HPLC method was developed for the determination of imidacloprid residue in different pH of water and soil. The Validation of analytical method for determination of imidacloprid residues by HPLC. The method consisted of extracting with methanol from soil. The extracts were subjected onto the column filled with florisil column chromatography. The extraction of imidacloprid residues from water with ethyl acetate. Quantification is performed by reversed phase HPLC with UV detector. The limit of quantitation (LOQ) was mg/kg 0.02 in soil and 0.02 mg/L in water. The limit of detection (LOD) was 0.01 mg/kg in soil and 0.01mg/L in water. Recoveries for imidacloprid were 95.18, 94.66, 95.27 and 94.78 % in black, red, sandy loam and clay soil respectively. Recoveries for imidacloprid were 96.86, 86.14, and 92.34 % in pH4, pH7, and pH9 respectively. The detector linearity and the repeatability of the method proved to be very precise.
全文可以在线浏览： http://www.eco-web.com/editorial/03588.html

Determination of imidacloprid in water and soil samples by gas chromatography-mass spectrometry
J. L. Vilchez et,al.
Journal of Chromatography A Volume 746, Issue 2, 11 October 1996, Pages 289-294
Abstract:
A method for determination of imidacloprid in water and soil samples, previous hydrolysis in basic medium, followed by gas chromatography-mass spectrometry and selected ion monitoring. A 250-ml sample water was previously heated in basic medium to give a hydrolysis compound of adequate volatility. The hydrolysis product which was extracted and isolated with chloroform was identified and found to be suitable for gas chromatography analysis. Further, a clean-up is not necessary using the selected ion monitoring mode. [2H10]Anthracene was used as an internal standard. The applicable concentration range was 5–20 μg l−1. Detection limit was 0.16 μg l−1 for water and 1 μg kg−1 for soil samples. Their relative standard deviations established for different concentration levels were between 0.3 and 1%. It was applied to the check whether there was imidacloprid above these limits on waters and soil from Granada (Spain). The method was validated applying the standard addition methodology. Recovery levels of the method reached 100% in all cases.

全文链接： http://www.sciencedirect.com/science?_ob=ArticleURL&_udi=B6TG8-3VVMN5D-K&_user=10&_rdoc=1&_fmt=&_orig=search&_sort=d&view=c&_acct=C000050221&_version=1&_urlVersion=0&_userid=10&md5=bec54d7e9015b849c98510359a9b2a68

小麦籽粒与土壤中吡虫啉残留测定
谢桂英, 杨洁, 劭丹丹
<<农药>>2006年 第45卷 第07期

Simultaneous determination of imidacloprid, thiacloprid, and thiamethoxam in soil and water by high-performance liquid chromatography with diode-array detection
YING Guang-Guo
Abstract
A high-performance liquid chromatography method with diode-array detection (HPLC-DAD) is described for the determination of three neonicotinoid insecticides imidacloprid. thiacloprid, and thiamethoxam in soil and water. The soil samples were extracted with acetonitrile, while the water samples were extracted using C18 cartridges. The mean recoveries plus standard deviations for spiked soil samples were 82±4.2% for thiamethoxam. 99±4.2% for imidacloprid and 94 ± 1.4% for thiacloprid. The recoveries for water samples ranged from 87±3.4% for thiamethoxam to 97 ±3.9% for imidacloprid and 97±2.6% for thiacloprid. The limits of quantitation (LOQ) were 0.1, 0.1, 0.01 mg/kg in soil (5g), and 2, 2, 11.5 μg/L in water (50 mL) for thiamethoxam, imidacloprid, and thiacloprid, respectively.

Journal of environmental science and health. Part B. Pesticides, food contaminants, and agricultural wastes；2004, vol. 39, no5-6, pp. 737-746 [10 page(s) (article)] (12 ref.)

为什么只有截图没有下载地址

dick523 发表:楼主，关于吡虫啉的分析方法，在论坛中已有讨论见链接:
http://www.instrument.com.cn/bbs/shtml/20070901/965432/
此外，有篇文章你可以参考：