这个标准里面没提吗？采用哪个标准方法呀？

操作没多大变化吧

毒死蜱不是一般都用在蔬菜上杀虫么

三重四级杆做定量比较好，普通离子阱一次只能进200000离子，进样量小了检测不到，进样量大了重复性差，你做物质的变化，我感觉量的变化是重要的检测目标，所以推荐三重四级杆，能用Q-TOF最好了

这样的响应差不多咯

我们报告出0.04ppm，但这只是一个自欺欺人的，根本达不到，不知道各位检不检测，怎样检测。

我们有检出过氯氰菊酯啊，不过小于0.01就是。

The new analytical method using Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) procedure for simultaneous determination of diacylhydrazine insecticide residues in fruits and vegetables was developed using ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS). The four insecticides (tebufenozide, methoxfenozide, chromafenozide, and halofenozide) were extracted from six fruit and vegetable matrices using acetonitrile and subsequently cleaned up using primary secondary amine (PSA) or octadecylsilane (C18) as sorbent prior to UPLC-MS/MS analysis. The determination of the target compounds was achieved in less than 3.0min using an electrospray ionization source in positive mode (ESI+) for tebufenozide, methoxfenozide, and halofenozide and in negative mode (ESI-) for chromafenozide. The limits of detection were below 0.6 gkg(-1), while the limit of quantification did not exceed 2 gkg(-1) in different matrices. The QuEChERS procedure by using two sorbents (PSA and C18) and the matrix-matched standards gave satisfactory recoveries and relative standard deviation (RSD) values in different matrices at four spiked levels (0.01, 0.05, 0.1, and 1mgkg(-1)). The overall average recoveries for this method in apple, grape, cucumber, tomato, cabbage, and spinach at four levels ranged from 74.2% to 112.5% with RSDs in the range of 1.4-13.8% (n=5) for all analytes. This study provides a theoretical basis for China to draw up maximum residue limits and analytical method for diacylhydrazine insecticide in vegetables and fruits.QuEChERS方法（C18、PSA）进行前处理。

前四种经常用到

样品冷冻和解冻的稳定性到是没有仔细考察过，不过当样品解冻时，如果解冻液流失再冻后样品在农残上不知道有没有损失。

还是说做回收?

国内的标准还是很混乱

大家继续支持

进出口检查，只要不合格，就不能出口，一次定生死。

建议优化一下SPE柱的方法:过SPE的时候，可以单独收集 上样液，淋洗液，和洗脱液，看看在那一部分损失的。 不同厂商的SPE柱可能有差异！

我们用的容量瓶就是有机溶剂超声，水超声，分析纯丙酮洗，色谱纯丙酮洗，然后晾干就行。

是不是这篇？

新霉素是不需要SPE柱的，直接提取就行了，但是用的色谱柱的是HILLIC

数据统计是一个比较繁琐的工作。

离心机，感觉还可以。左边有一颗螺丝有问题，容易滑出来，影响使用，需要小心