Application of porous membrane protected micro-solid-phase-extraction combined with gas chromatography-mass spectrometry for the determination of estrogens in ovarian cyst fluid samples.
A cost effective and environmentally friendly extraction technique using porous membrane protected micro-solid phase extraction (μ-SPE) is described for the extraction of estrogens in cyst fluid samples obtained from cancer patients. A sorbent (ethylsilane (C2) modified silica) (20 mg) was packed in a porous polypropylene envelope (2 cm×1.5 cm) whose edges were heat sealed to secure the contents. The μ-SPE device was conditioned with acetone and placed in a stirred (1:5) diluted cyst fluid sample solution (10 mL) to extract estrogens for 60 min. After extraction, the analytes were desorbed and simultaneously derivatized with a 5:1 mixture of acetone and N,O-bis(trimethylsilyl)-trifluoroacetamide. The extract (2 μL) was analyzed by gas chromatography-mass spectrometry. Various extraction, desorption and derivatization conditions were optimized for μ-SPE. With this simple technique, low limits of detection of between 9 and 22 ng L(-1) and linear range from the detection limits up to 50 μg L(-1) were achieved. The optimized method was used to extract estrogens from cyst fluid samples obtained from patients with malignant and benign ovarian tumors.
Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore.
Sivarajan
S
Kanimozhi
Chanbasha
C
Basheer
Kothandaraman
K
Narasimhan
Lin
L
Liu
Stephen
S
Koh
Feng
F
Xue
Mahesh
M
Choolani
Hian Kee
HK
Lee
D000081:Acetamides / Q000737:chemistry; D000096:Acetone / Q000737:chemistry; D020420:Cyst Fluid / Q000737:chemistry*; D004967:Estrogens / Q000032:analysis* / Q000302:isolation & purification; D005260:Female; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D010051:Ovarian Neoplasms / Q000378:metabolism; D010053:Ovary / Q000378:metabolism; D016062:Porosity; D052617:Solid Phase Microextraction / Q000379:methods*; D014297:Trimethylsilyl Compounds / Q000737:chemistry
D000081:Acetamides; D004967:Estrogens; C103255:N,O-bis(trimethylsilyl)trifluoroacetamide; D014297:Trimethylsilyl Compounds; D000096:Acetone