Solid-phase extracted (Oasis HLB cartridge) wastewater samples were preserved in methanol for HPLC-MS-MS analysis at -20°C. After a lapse of 3 months, I see some of the extracted samples show turbidity/flocculation.  What could be the reason?  Further, what steps do I need to take (for eg. filtration) before injecting it to the LC-MS?  

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