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Pyrethroids in Blood Plasma and Urine 27 Table 4 Precision in Series and Detection Limits of Pyrethroids Plasma 0.1 Plasma 1.0 Detection µg/L µg/L limit Pyrethroid R.S.D. (%) R.S.D. (%) (ng/L) Bioallethrin 10.5 17.5 5 Permethrin (sum of 2 isomers) 8.4 16.9 5 Cyfluthrin (sum of 4 isomers) 9.9 9.4 5 Cypermethrin (sum of 4 isomers) 6.4 10.8 5 Deltamethrin RSD, relative standard deviation. 15.1 10.3 20 13. Combine organic layer in the new screw cap test tube (step 9). 14. Discard the lower urine phase. 15. Dry organic layer under a gentle stream of nitrogen just to dryness. 16. Dissolve residue in 250 µL acetonitrile. 17. Add 30 µL of HFIP (see Note 10). 18. Add 20 µL of DIC. 19. Derivatize solution under slight mixing for 10 min at room temperature. 20. Add 1 mL 1 M sodium hydrogen carbonate solution. 21. Add 250 µL iso-octane. 22. Cover test tube and mix sample 10 min vigorously for extraction. 23. Centrifuge sample 5 min at 2000 for phase separation. 24. Separate iso-octane phase in a microvial. 3.2.2. Operational Parameters for GC and MS 3.2.2.1 GC PARAMETERS Use HP 5890II with SSL-Injector and CTC A 200S Autosampler. Rtx 65.30 m × 0.25 mm × 0.25 µm column He 120 kPa for 1 min, 100 kPa/min, 80 kPa gas pressure 1 min off purge time 40-mL/min split 3-mL/min septum purge 60°C 1 min >8°C/min >150°C >30°C/min at 300°C for 20 min 300°C injection temperature 1 µL injection volume 3.2.2.2. MS Parameters Use a Micromass AutoSpec Ultima. 250°C interface. 250°C source. EI mode inner source (see Note 11). 0.3-mA filament. 70 eV electron energy. Maximum 8000 accelerating voltage. 330-V multiplier.
28 Leng and Gries Table 5 SIM Masses and Retention Time for MS Detection of Pyrethroid Metabolites (HFIP-Ester) in Urine Pyrethroid metabolite Target mass (m/z) Retention time (min) cis -CDCA 331.077 7:19 trans-CDCA 331.077 6:21 cis-DCCA 323.027 7:34 trans-DCCA 323.027 7:45 cis-DBCA 368.975 10:52 2-PBA (internal standard) 364.053 14:27 3-PBA 364.053 14:39 FPBA 382.044 14:05 10,000 resolution. Perfluorokerosine calibration gas 3.2.3. Analytical Determination Inject 1 µL of the sample (sample preparation, step 24) into the GC–MS system. If the instrument parameters are set as described in Subheading 3.2.2. in SIM EI + mode (Table 5), a stereoselective resolved chromatogram of each pyrethroid metabolite can be obtained as shown in Fig. 5. This sample can optionally be analyzed in NCI mode as shown in Fig. 6 (see Note 11). 3.2.4. Method Validation The calibration curve and the samples for precision control are prepared with urine of persons not exposed to pyrethroids. Necessary fortification levels for this procedure were prepared in agreement with the fortification levels in Table 2. The linearity of all pyrethroid metabolites is tested in a range between 0.1 and 100 µg/L urine, with correlation coefficients more than 0.995. If the method is working correctly, quality criteria for precision in series can be achieved as listed in Table 6. The average recovery of all compounds lies between 90 and 100%. 3.2.5. Storage Stability The starting solutions and stock solutions can be stored in a deep freezer at −18°C for at least 6 mo. Longer times were not tested. Urine samples can be stored for more than a year at −21°C in a deep freezer 4. Notes 1. This method is developed for the determination of very low pyrethroid concentrations in blood plasma, which are caused by the short pyrethroid half-lives in blood plasma. Therefore, this method is useful for the determination of pyrethroids following acute intoxication. 2. Several analytical techniques have been tested previously, but all gave poor reproducibilities or sensitivities. A direct extraction with iso-octane after precipitation with sodium chloride and ethanol also works, but only for a few samples. In such a plasma extract,
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2,4-D and MCPA in Human Urine 91 7
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2,4-D and MCPA in Human Urine 93 4.
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2,4-D and MCPA in Human Urine 95 Ta
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2,4-D and MCPA in Human Urine 101 F
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106 Jardim, Pozzebon, and Queiroz S
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108 Jardim, Pozzebon, and Queiroz 3
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110 Jardim, Pozzebon, and Queiroz A
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112 Zhang been widely used to detec
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114 Zhang 3. Maintain the ion sourc
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116 Zhang Fig. 1. Mass ion chromato
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118 Zhang 15. Crespin, M. A., Galle
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120 Knopp The search for alternativ
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122 Knopp 4. Dissolve 40 mg BSA in
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124 Knopp Fig. 2. Scheme of tracer
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128 Knopp Fig. 4. Phenoxyalcanoic a
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130 Knopp 18. No or only minimal sa
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HTS-IS-ELISA for Biomonitoring Chlo
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166 Glass the collector and the mom
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168 Glass 3.2.1. Selection of Appli
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170 Glass Fig. 2. A field layout fo
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172 Glass questions that may arise
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174 Glass 3.5.3. Labeling of Media
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176 Glass Again, this can be relate
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Determination of Insecticides in In
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185 Fig. 3. Total ion current (TIC)
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187 Fig. 5. TIC chromatogram (y-axi
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Exposure to Malathion and Metabolit
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Internal Quality Criteria 219 17 Qu
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Internal Quality Criteria 221 instr
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223 Fig. 1. Basic components of the
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Internal Quality Criteria 225 Fig.
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Internal Quality Criteria 227 Resul
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Internal Quality Criteria 229 5. Th
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Pesticide Analysis by ELISA 231 18
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Pesticide Analysis by ELISA 233 4.
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QuEChERS Approach for Pesticides 23
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253 Table 2 Conditions for the GC-M
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268 Di Muccio et al. Table 1 Mean (
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270 Di Muccio et al. evaporator. In
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Pesticide Analysis by LPGC-MS/MS 27
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286 Barker shorten turnaround time,
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288 Barker 9. The extract is placed
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290 Barker The mobile phase composi
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292 Barker phase solid support surf
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294 Barker 8. Fernandez, M., Pico,
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296 Barker 43. Pico, Y., Molto, J.
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298 Picó ultraviolet absorbance, i
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300 Picó 3. Attach the conditioned
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302 Picó Fig. 2. EDA-only vs conve
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304 Picó Fig. 3. CE-MS/ESI electro
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306 Picó Fig 4. CE-MS/ESI electrop
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308 Picó tration. The optimum samp
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320 Papadopoulou-Mourkidou, Papadak
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326 Table 4 Method Validation Data:
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α-Hexachlorocyclohexane in Food 33
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Screening of Pesticides by HS-SPME-
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LC/LC for Pesticide Analysis 383 29
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LC/LC for Pesticide Analysis 385 Fi
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LC/LC for Pesticide Analysis 389 re
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LC/LC for Pesticide Analysis 391 4.
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LC/LC for Pesticide Analysis 399 sa
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LC/LC for Pesticide Analysis 403 19
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Analysis of Organotins by GC-HRMS 4
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Triazine in Water 467 34 Determinat
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Triazine in Water 469 with various
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Triazine in Water 471 Fig. 1. A chr
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Triazine in Water 473 Fig. 2. LC/AP
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475 Table 3 General Conditions Used
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Triazine in Water 477 (>60%) except
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Triazine in Water 479 13. Koskinen,
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482 Rodríguez-Mozaz, López de Ald
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Index 491 Index Adipose tissue anal
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Index 493 high-throughput screening
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Index 495 Food analysis, see Atrazi
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Index 497 HPLC, see High-performanc
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Index 499 quality control, 98 recov
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Index 501 Pyrethroids, air sampling
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Index 503 Uncertainty, estimation,
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