Screening of Pesticides in Water with LC–MS–MS Using On-line SPE

Mar 02, 2014

Pesticides are widely used in agriculture to protect crops from insect infestation. An important application of this equipment is the possibility to analyze pesticides in water without pretreatment of the sample. Shimadzu has developed a system for injection of water samples using Nexera with LCMS-8030 including on-line solid-phase extraction (SPE).

Pesticides are widely used in agricultural products to protect crops from insect infestation during cultivation and product transport. The abuse of pesticides can cause significant environmental pollution in many areas, especially at the level of lakes, rivers, and aquifers. For this reason, one of the most important and attractive applications is the ability to analyze pesticides in water without pretreatment of the sample. In cooperation with Arpa Asti (Italy), Shimadzu developed a system for injection of water samples using a LCMS-8030 triple quadrupole in combination with a Nexera UHPLC instrument with on-line solid-phase extraction (SPE) to identify a mixture of 48 substances.

Materials and Methods


Figure 1: Schematic design and flowline diagram of the Shimadzu solution for an on-line SPE and conventional UHPLC analysis within one system.
A standard mixture of pesticides was used for optimization of all multiple reaction monitoring (MRM) parameters. A 1 mL amount of previously filtered sample was injected directly and an on-line SPE column was applied for concentration. The design of the system allows switching between different injection volumes within one instrument configuration, which is completely controlled by the Shimadzu LabSolutions Software (Figure 1). With a single autosampler it is therefore possible to inject up to 50 µL volume for conventional UHPLC analysis and up to 2 mL sample volume for the analysis with on-line SPE pre-concentration.

Analytical Conditions





Figure 2: Calibration curves of metamitron and cloridazon and examples of real sample injection using on-line SPE.
The Shimadzu LCMS-8030 was applied in MRM mode for detection of the researched compounds. For construction of a calibration curve water samples spiked with a standard were used. Figure 2 shows two exemplary calibration curves of metamitron and cloridazon from a total of 48 substances, all in a concentration range from 0.002 µg/L to 0.100 µg/L, and two different examples of real sample injections using on-line SPE.


The new LCMS-8050 — speed and sensivity beyond comparison.
In addition to the on-line SPE option with large volume injection for pesticides in water, the system can be used as an UHPLC instrument for low volume injections applying the same autosampler to reduce costs and the number of systems.

The UFMS series (Ultra Fast Mass Spectrometry) from Shimadzu not only provides extremely high speed analysis but also impressive high sensitivity, to meet the growing demand for trace-level quantitation in various application fields. The newest member of the UFMS-family, the LCMS-8050 features the world's fastest data acquisition rates and best-in-class sensitivity. Method transfer of other models (LCMS-8030 and LCMS-8040) can easily be adopted.


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