Page 38 - LC-SFC_Pharma_Brochure

5. Using the Nexera UC SFE Pretreatment The pesticide standard solutions were added to an brown rice sample
System for the Extraction of Residual (pesticide concentrations of 100 ng/g). An MRM chromatogram of
Pesticides from Agriproducts the extraction liquid obtained from this sample is shown in Fig. 7. The
theoretical concentration of each pesticide in the extraction liquid
used for GC/MS/MS analysis was 50 ng/mL.
Over 800 pesticides are subjected to analysis for their residual presence
in food products. Analytical methods that enable rapid and simple test- The extraction was performed on six samples to which the abovemen-
ing of a large number of pesticides involving any pretreatment opera- tioned pesticide standard solutions were added; each pesticide was
tions required for analysis are needed. Conventional analysis for residu- quantiÿed using a matrix calibration curve created using the SFE extrac-
al pesticides in food normally involves a solvent extraction method to tion liquid obtained from a blank brown rice sample, after which re-
extract the pesticides, followed by LC/MS or GC/MS analyses. The pre- peatability and recovery were conÿrmed. Good repeatability (relative
treatment operations employed in these analytical methods are highly standard deviation of quantiÿed concentration: <10 %) and good re-
labor and time consuming, and they use a large volume of organic sol- covery (70 %–120 %) were obtained for the 301 pesticides studied. An
vent. We present an example of utilizing the Nexera UC SFE pretreat- excerpt from these results showing the repeatability and recovery for
ment system to extract residual pesticides before analyzing them using some representative pesticides is shown in Table 6. The Nexera UC SFE
a GC/MS/MS system. 1 g of dehydrating agent was added to 1 g of pul- pretreatment system can be used for automated consecutive pretreat-
verized brown rice*. This mixture was then enclosed into an extraction ment of up to 48 samples while consuming low amounts of solvent.
vessel, and an extraction pretreatment was performed using the condi-
tions shown in Table 4. The extraction liquid recovered by the fraction Table 5 Conditions Used for the Analysis of
collector was diluted to 2 mL with an acetone/hexane (1/1, V/V) mixture the Pretreated Samples (GC/MS/MS)
in a measuring ‚ask and then analyzed using GC/MS/MS under the Column : Rxi-5Sil MS 30 m × 0.25 mmI.D., df = 0.25 £m
conditions shown in Table 5. The components included in pesticide Column temp. : 50°C (1 min) ĺ (25°C/min) ĺ 125°C
standard mixture solutions for GC/MS (PL2005 Pesticide GC/MS Mix I ĺ (10°C/min) ĺ 300°C (15 min)
to VI and Mix 7, Hayashi Pure Chemical Ind., Ltd.) were analyzed. Carrier gas : He (Constant linear velocity mode)
* "Miyazaki Hydro-Protect" Patent No. 3645552 Linear velocity : 47.2 cm/sec
Injection mode : Splitless (Sampling time 1.00 min)
Table 4 SFE Conditions High press inj. : 250 kPa (1.5 min)
Injection volume : 1 £L
Of ine SFE Interface temp. : 250°C
Extraction vessel : 5 mL Ion source temp. : 200°C
Extraction solvent : CO2 + Methanol MS mode : MRM
Flow rate : 5 mL/min Loop time : 0.3 sec
Temperature : 40°C
Back pressure : 15 MPa
Extraction time : 8 min (Static extraction ĺ Dynamic extraction) Table 6 Repeatability and Recovery of Representative Pesticide Extraction
Trap & Pressure down conditions Repeatability Recovery
Compounds
Trap column : Shim-pack VP-ODS 4.6 mmI.D. × 50 mmL. 5 £m (%RSD, n=6) (%)
Temperature : 60°C Cyhalofop-butyl 4.2 93
Pressure down time : 4 min (8–12 min)
Etofenprox 3.8 90
Recovery conditions
Iprodione 2.5 93
Elution solvent : Acetone/Hexane = 1/1 (V/V)
Flow rate : 2 mL/min Malathion 3.2 93
Fraction time : 2 min (12–14 min) Piperonyl butoxide 3.8 89

(×1,000,000)
1.5
1.0

0.5 Fig. 7 MRM Chromatogram
of the Brown Rice
Extraction Liquid
0.0
3. 0 4 .0 5. 0 6 .0 7. 0 8 .0 9.0 10.0 11.0 12.0 13.0 14.0 15.0 16.0 17.0 18.0 19.0 20.0 21.0 22.0 23.0 24.0

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