Pesticide Residues in Milk and Milk Products - Pesticides: Evaluation of Environmental Pollution - page 582

TABLE 18.3
Residual Analysis of Pesticides In Milk and Milk Products (Selected Methods)

Analytical
System

Recovery
(%)

LOD
( µ g/kg) Analyte Extraction Separation References

Organochlorine
pesticides

Extraction with
petroleum ether

Capillary
DB-5
column

GC-ECD 91.0-99.1 0.01-0.03 Waliszewski

et al. (1997)

Organochlorine
pesticides

Cleanup of
hexane extract
with official
method

DC-200
Packed on
chromosorb

GC-ECD 84.5-98.2 1 Losada et al.

(1996)

Herbicides and
fungicides

SPE extraction C-18 LC-MS 82-120 0.008-1.4 Bogialli et al.

(2006)

Organochlorine
pesticides

Acetonitrile
petroleum ether
followed by
Florisil cleanup

HP-1
Capillary
column
30 m length

GC-ECD 90-94 1 Abou Donia

et al. (2010)

Cypermethrin,
fipronil,
chlorfenvinphos

QuEChERS
(MSPD)

GC-MS DB-5

Capillary
column

70-120 20 Brondi et al.

(2010)

Organochlorine
pesticides in
butter

Extraction with
hexane
partitioned with
acetonitrile and
dichloromethane

GC-ECD Chromosorb

OV-17

85-92 100 Gill et al. (2009)

48 compounds in
milk

Acetonitrile
acetone

UPLC/
Q-TOF and
GC-MS/MS

C-18,
2.1 × 100 mm
and ZB-50

70-85
70-100

— Hakala et al.

(2009)

New technologies such as SPE, SPME, and MSPD are suitable to perform extraction and
cleanup in a single step.

18.7.4 Separation and Detection

The quantification of the target analytes is usually performed with gas chromatography or
liquid chromatography separation, followed by detection using various detectors.
Gas chromatography appears to be the most useful technique for the quantitative deter-
mination of pesticide residues in milk and milk products.
Possible detectors in combination with GC are electron capture detector (ECD), therm-
ionic detectors such as nitrogen and phosphorus detector (NPD), flame photometric detec-
tor (FPD) or flame ionization detector, and mass selective detector (MSD).
High-performance liquid chromatography is the second most frequently used tech-
nique to determine very polar and low volatile pesticides. The separation mostly occurs
on reverse-phase packed columns. Different types of detectors for HPLC to determine pes-
ticide residues are UV absorption, fluorescence, conductivity, electrochemical, and mass
spectrometer detectors.
Liquid chromatography, along with a mass selective detector (MSD), is a very powerful
technique for the quantification and confirmation of pesticide compounds (see Bogialli
and Di Corcia (2010) for further details).