MLA-068 Rev 3 GC-MS Analysis of Hormones and

Sterols

Bharat Chandramouli05-August-2009

What’s New? Method Emphasis

– The method is primarily intended for the low level detection of hormones and sterols in aqueous samples (low organic particulate content), and low organic solids not associated with wastewater treatment.

– Options available for higher level samples including biosolids

– Currently, “clean water” or “ultra-trace” options under development, removed from method

Method Emphasis Choices

– Low level hormones + sterols in low organic matrices – Suitable, cholesterol and sitosterol may be estimated values

– Low level Hormones in biosolids/influents – MLA-072 is more appropriate

– Sterols in high organic matrices – Suitable, but under dilution and split conditions that may compromise hormones detection limits

Samples Preferred Samples

– Potable water– Surface water– Ground water– POTW Final Effluent– Non-TCLP leachates– Sediments, low organic soil

Method Emphasis Important to know sample origin, and

client expectations on relative importance of analytes.

Hormones or Sterols? Any particular hormones to emphasize?

This knowledge will drive method choices

Method Emphasis Sterols

– May be reported as estimated concentrations if calibration range is exceeded, especially in biosolids samples

– Specific client request will supersede this default option

Extraction Water

– All water samples will be filtered– Default option is filtrate only– Whole water – Filtrate + solids available – Extraction procedure similar to MLA-072

Solids– 1g default sample size: 5g wet maximum– Sonication in buffered methanol

Cleanup Oasis HLB for water and solids LAF and other column cleanups retired Current estimate – 3 days from

preparation to instruments

Analysis and Reporting Ergosterol now information only, no criteria

attached 4 analytes testosterone, androsterone,

androstenedione and desogestrel against recovery standard– Note: Non-estrogens do not perform well against

the estrogen surrogate 17β-Estradiol-d4 New acceptance criteria for recovery –

QDO-015 recovery estimates do not apply