title: [Simultaneous identification and detection of 16 anabolic steroid hormones in muscle using liquid chromatography oupled to quadrupole/linear ion trap mass spectrometry].
abstract: A comprehensive method for simultaneous identification and detection of 16 anabolic steroid hormones (ASs, including andorgens, gestagens and their esters) in muscle samples was developed with liquid chromatography coupled to quadrupole/linear ion trap mass spectrometry (LC-Q/Trap-MS). The ASs in muscle samples were extracted with acetonitrile under ultrasonic assistance. The extract was defatted by n-hexane with liquid-liquid partitioning and followed by clean-up with NH2 solid phase extraction (SPE) cartridge. The separation of analytes was carried out on a CAPCELL PAK C18 MG II column (150 mm x 2.0 mm, 5.0 microm) using mobile phases of 0.1% (v/v) formic acid in acetonitrile and 0.1% (v/v) formic acid-5 mmol/L ammonium formate aqueous solution with gradient elution. A scheduled multiple reaction monitoring (sMRM) in positive mode as survey scan and an enhanced product ion (EPI) scan as dependent scan in an information-dependent acquisition (IDA) experiment was adopted in mass spectrometry acquisition. On-line lab-built MS/MS library and internal standards were employed for the identification and quantification. As a result, the 16 ASs showed good linearity with all correlation coefficients (r) no less than 0. 999 0 within the linear ranges. The limits of quantification (LOQs, S/N > or = 10) for the 16 ASs were in the range of 0.029-0.36 microg/kg. At the three spiked levels (0.5, 2.0 and 20 microg/kg), the overall recoveries ranged from 89.9% to 118% with the relative standard deviations (RSDs) no more than 16.2% under within--laboratory reproducibility conditions. The proposed method can be used to identify and detect the 16 ASs in a single run, which makes it effective in residue surveillance of anabolic hormones in muscle samples.
authors: Technical Center of Entry-Exit Inspection and Qurantine, Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266002, China. light04@126.com
authors: Hongwei'
authors: H
authors: Zhang
authors: Xue
authors: X
authors: Cai
authors: Liming
authors: L
authors: Lin
authors: Liangzhen
authors: L
authors: Chen
authors: Chengzhu
authors: C
authors: Liang
authors: Lei
authors: L
authors: Bao
authors: Zhixu
authors: Z
authors: Tang
authors: Zengyuan
authors: Z
authors: Niu
authors: Fengmei
authors: F
authors: Wang
mesh_terms: D045930:Anabolic Agents / Q000032:analysis; D000728:Androgens / Q000032:analysis; D000818:Animals; D002853:Chromatography, Liquid / Q000379:methods*; D005506:Food Contamination / Q000032:analysis*; D012739:Gonadal Steroid Hormones / Q000032:analysis*; D018482:Muscle, Skeletal / Q000737:chemistry*; D011372:Progestins / Q000032:analysis; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*
chemical_list: D045930:Anabolic Agents; D000728:Androgens; D012739:Gonadal Steroid Hormones; D011372:Progestins