主题：【求助】吡嘧磺隆残留量的测定方法

附件请参考。

感谢雾非雾的意见，可是我要的是农药残留的分析方法，不是有效成分的分析方法。

看日本农用化学品多残留一齐分析法LCMSII法的粒子信息表中有这个农药，可以用LCMSII法试试。

原文由 雾非雾(mcds) 发表:
看日本农用化学品多残留一齐分析法LCMSII法的粒子信息表中有这个农药，可以用LCMSII法试试。

以上的方法是多残留分析，请问能否把此方法的链接或是网址给一下小弟我。

论坛里的相关链接如下：
日本厚生劳动省-食品中残留农药兽药饲料添加剂检测方法
出自：【求助】－日本厚生劳动省-食品中农用化学品残留检测方法  2楼
http://www.instrument.com.cn/bbs/shtml/20060609/454290/

“日本食品中农业化学品残留检测方法”
  http://www.instrument.com.cn/bbs/download.asp?ID=16309
出自：【求助】大豆的前处理方法  3楼
http://www.instrument.com.cn/bbs/shtml/20090318/1791998/

日本食品中农业化学品残留检测方法
http://www.instrument.com.cn/bbs/shtml/20060406/384588/

原文由 雾非雾(mcds) 发表:
论坛里的相关链接如下：
日本厚生劳动省-食品中残留农药兽药饲料添加剂检测方法
出自：【求助】－日本厚生劳动省-食品中农用化学品残留检测方法  2楼
http://www.instrument.com.cn/bbs/shtml/20060609/454290/

“日本食品中农业化学品残留检测方法”
  http://www.instrument.com.cn/bbs/download.asp?ID=16309
出自：【求助】大豆的前处理方法  3楼
http://www.instrument.com.cn/bbs/shtml/20090318/1791998/

日本食品中农业化学品残留检测方法
http://www.instrument.com.cn/bbs/shtml/20060406/384588/

不过没有吡嘧磺隆这个产品农药的残留分析，但还是很感谢！

原文由 kekemi(kekemi) 发表:

原文由 雾非雾(mcds) 发表:
论坛里的相关链接如下：
日本厚生劳动省-食品中残留农药兽药饲料添加剂检测方法
出自：【求助】－日本厚生劳动省-食品中农用化学品残留检测方法  2楼
http://www.instrument.com.cn/bbs/shtml/20060609/454290/

“日本食品中农业化学品残留检测方法”
  http://www.instrument.com.cn/bbs/download.asp?ID=16309
出自：【求助】大豆的前处理方法  3楼
http://www.instrument.com.cn/bbs/shtml/20090318/1791998/

日本食品中农业化学品残留检测方法
http://www.instrument.com.cn/bbs/shtml/20060406/384588/

不过没有吡嘧磺隆这个产品农药的残留分析，但还是很感谢！

因为现在能找到的日本一齐分析法的版本都是06年检验检疫科学院翻译的，后来又有一个增补本（此版没见到电子版），我们从日本官方网站上复制的检测项目及相关粒子信息表上，是LCMSII法可以检测，您可以按这个方法试试。

Determination and Quantitation of Ten Sulfonylurea Herbicides in Soil Samples Using Liquid Chromatography with Electrospray Ionization Mass Spectrometric Detection

Abstract

A multiresidue method was developed for confirmation and quantitation of ten sulfonylurea herbicides including nicosulfuron, thifensulfuron-methyl, metsulfuron-methyl, sulfometuron-methyl, chlorsulfuron, ethametsulfuron-methyl, tribenuron, bensulfuron-methyl, pyrazosulfuron-ethyl, and chlorimuron-ethyl in soil. Analytes were extracted from the soil sample with methanol-phosphate buffer (2:8, v/v) (pH 7.8) in an ultrasonic bath. The extracts were adjusted to pH 2.5 with 85% H₃PO₄ and passed, under vacuum, through a solid-phase extraction cartridge. Several types of adsorbents were evaluated, including silica-based Cleanert C₁₈ and two polymeric adsorbents (Oasis HLB and Cleanert HXN). Cleanert C₁₈ showed good cleanup effects in the study. Determination and quantitation were performed by high performance liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) instrumentation equipped with an ion trap mass filter. Analytes were eluted on a HPLC column of 4.6 mm × 250 mm XDB C₁₈, 5 × particle size, in the mobile phase of the acetonitrile (solvent A)-methanol (solvent B)-0.2% acetic acid (solvent C). The elution gradient was as follows: the mobile phase started with 10% of acetonitrile and 10% methanol, which increased linearly to 45% in 14 min, to 48% in the next 2 min and then returned to the initial condition in 2 min. The column temperature was kept at 30°C with a flow rate of 1.0 ml/min. Thus the retention time of nine herbicides was in the range of 10 to 16 minutes. Spiked soil at 0.01–1.0 mg/kg levels was checked. Average recoveries were in the range of 80.2%–104.5% with relative standard deviations (RSDs) of 0.02%–14.90%. The limit of detection (LOD) of this method was in the range of 0.6 to 3.5 μg/kg.

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http://www.sciencedirect.com/science?_ob=ArticleURL&_udi=B82YT-4NRMT49-1&_user=10&_coverDate=09%2F30%2F2006&_rdoc=1&_fmt=high&_orig=search&_sort=d&_docanchor=&view=c&_searchStrId=1423173671&_rerunOrigin=google&_acct=C000050221&_version=1&_urlVersion=0&_userid=10&md5=fd06001ebbf6074aef53c558413051fb

SNT 2325-2009 进出口食品中四唑嘧磺隆、甲基苯苏呋安、醚磺隆等45种农药残留量的检测方法 高效液相色谱-质谱 质谱法

液相色谱法同时测定下13种磺酰脲类除草剂