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Autospec ultima

Manufactured by Waters Corporation
Sourced in United Kingdom

The Autospec Ultima is a high-performance liquid chromatography (HPLC) system designed for analytical and preparative applications. It features a variety of modules, including a solvent delivery system, an autosampler, a column oven, and a UV-visible detector. The Autospec Ultima is capable of performing a wide range of HPLC techniques, such as normal-phase, reversed-phase, and ion-exchange chromatography.

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3 protocols using autospec ultima

1

Dioxin and PCB Determination Protocol

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PCDD/Fs and PCBs were determined using a high-resolution gas chromatographer (Agilent 6890N, Wilmington, NC, USA) coupled with high-resolution mass spectrometer (AutoSpec Ultima, Waters Micromass, Wilmslow, UK) (HRGC/HRMS). Chromatographic separation was achieved on a DB-5MS fused silica capillary column (60 m × 0.25 mm i.d. × 0.25 μm, Agilent, USA). The mass spectrometer was operated in positive electron impact (EI+) and the targets were analyzed in voltage selective ion records (VSIR) mode at a mass resolution of above 10,000. The electron energy was 35 eV, and the ion source and transfer line were kept at 270 °C. Helium was used as the carrier gas at a flow rate of 1 mL min−1. The injection port temperature was held at 270 °C and 1 μL of the sample was injected into the GC in splitless mode. The GC oven temperature was programmed as follows: for PCBs, the initial temperature was 120 °C, held for 1 min, and then increased to 150 °C at a rate of 30 °C min−1, ramped to 300 °C at 2.5 °C min−1 and held for 1 min; for PCDD/Fs, 150 °C for 3 min, 20 °C min−1 to 230 °C and held for 18 min, increased to 235 °C at 5 °C min−1 and held for 10 min, and finally 4 °C min−1 to 330 °C and held for 3 min. Seventeen 2,3,7,8-substituted PCDD/F congeners, twelve dioxin-like PCB congeners, six indicator PCB congeners and six other PCB congeners were determined.
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2

Determination of Persistent Organic Pollutants

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Serum concentrations of 6 PCB congeners (PCB118, PCB153, PCB138, PCB156, PCB170 and PCB180), DDE and HCB were determined by means of a Agilent 6890 gas chromatographer connected to a Waters Autospec Ultima high resolution mass spectrometer as described in an earlier study on the exposure data12 (link), 13 (link). Per subject we calculated a Z-Score(POPs) as a representative of the internal exposure to the mixture of POPs. The Z-Score(POPs) was defined as the sum of the Z-Scores for each compound: Z-Score(compound) = (X − μ)/σ (where X represents the value of the subject, μ the mean and σ the standard deviation of the population)42 (link). Therefore, Z-Score(POPs) = Z-Score(PCB118) + Z-Score(PCB153) + Z-Score(PCB138) + Z-Score(PCB156) + Z-Score(PCB170) + Z-Score(PCB180) + Z-Score(HCB) + Z-Score(DDE).
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3

GC-MS Analysis of Electrophysiologically Active Compounds

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Electrophysiologically active GC peaks were analysed using a 50 m × 0.32 mm ID HP-1 column (J & W Scientific), equipped with a cool on-column injector, that was coupled to a Waters Autospec Ultima magnetic sector mass spectrometer (Waters Corp., Manch-ester, UK). Ionization was by electron impact at 70 eV and 220 ∘ C. The GC oven temperature was maintained at 30 ∘ C for 1 min, then programmed at 5 ∘ C/min to 150 ∘ C and held for 0.1 min, then pro-grammed at 10 ∘ C/min to 250 ∘ C and held for 34.9 min. Tenta-tive identifications were made by comparison of mass spectra to those contained in a library database, 35 and confirmed by GC peak enhancement using authentic samples of compounds purchased from commercial suppliers.
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