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Multi-component quantitative analysis of pharmaceuticals and personal care products in the environment by LC-MS/MS with fast polarity switching Natsuyo Asano, Kiyomi Arakawa, Shinjiro Fujita, Multi-component quantitative analysis of pharmaceuticalsand personal care products in the environment by LC-MS/MS with fast polarity switching IntroductionPharmaceuticals and personal care products (PPCPs) that are able to analyze multiple classes of compound constitute a group of emerging contaminants which have within one analytical procedure. Here we report a new received considerable attention in recent years. Monitoring multi-residue UHPLC-ESI-QqQ method that utilizes fast of PPCPs in the environment is vital as many of these polarity switching with an optimized chromatographic compounds are ubiquitous, persistent and biologically gradient that removes matrix effects and results in excellent active with recognised endocrine-disruption functions. ng/L detection levels. Furthermore, we have evaluated the Given the hazardous nature of these compounds, there is a performance of polarity switching in comparison to need to provide fast and sensitive multi-residue methods Materials and MethodsNatural river and lake water was collected from the Shiga pre-treatment, at a range of concentration levels (1 - region (Japan) and spiked, without any sample Shim-pack XR-ODSIII (2.0 mmI.D. x 50 mmL., 1.6 µm) 0%B (0-6 min) - 80%B (16 min) - 100%B (16.01-18 min) - 0%B (18.01-21 min) A higher sensitivity triple quadruple mass spectrometer with fast polarity switching (20 msec) was used for the (LCMS-8080, Shimadzu, Japan) operating in SRM mode detection of positively and negatively charged analytes. Multi-component quantitative analysis of pharmaceuticalsand personal care products in the environment by LC-MS/MS with fast polarity switching ResultsAnalysis of PPCPs spiked in environmental waterAs a result of the complex matrix in which PPCPs are analytes at the head of the chromatographic column while present, the occurrence of ion suppression/enhancement allowing the interfering environmental matrix to be eluted can reduce MS/MS detection limits. For this reason, an optimized gradient was developed that focused target Before the organic phase was increased, the aqueous mobile phase held at 100% for 6 min. All compounds were measured by SRM with fast polarity linearity (R2 > 0.999). The analysis results of 15 PPCPs are switching (20 msec) for multi-component analysis. Excellent shown in Table 2, Fig. 2 shows calibration curves for three limits of quantification were achieved in the range 1 - 50 selected PPCPs: Carbamazepine, Albeterol and Ibprofen.
ng/L for nearly all studied compounds, with outstanding Table 2 MRM mode parameters and analysis results for each PPCPs. Multi-component quantitative analysis of pharmaceuticalsand personal care products in the environment by LC-MS/MS with fast polarity switching Fig. 2 Calibration curves for Carbamazepine (a), Albeterol (b) and Ibprofen (c); (a) was spiked in river water, (b) and (c) were spiked in lake water.
Polarity SwitchingTo evaluate the capability of polarity switching the data quality obtained was compared to dedicated positive or Long term stability was investigated by making 100 injections over 10 hours. Polarity switching data indicates Data quality obtained during polarity switching experiments excellent stability over the analysis time (Fig. 4, Table 3). was directly comparable to that achieved during dedicated Fig. 3 Comparison of polarity switched analysis (a) and non-polarity switched analysis (positive only or negative only analysis) (b).
Fig. 4 Results for area variation across the 100 serial analyses.
Multi-component quantitative analysis of pharmaceuticalsand personal care products in the environment by LC-MS/MS with fast polarity switching Table 3 Analysis results for respective compounds.
Optimization of the LC gradient program resulted in the reduction of matrix effect and the recoveries of 70 - 120% for almost all studied compounds.
Using LCMS-8080, excellent sensitivity and linearity were obtained for PPCPs spiked in environmental water samples.
Fast polarity switching results were shown to be comparable to dedicated single polarity experiments for the analysis of PPCPs in environmental samples.
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