PMID- 23383485 OWN - NLM STAT- MEDLINE DCOM- 20140502 LR - 20190923 IS - 1000-8713 (Print) IS - 1000-8713 (Linking) VI - 30 IP - 10 DP - 2012 Oct TI - [Simultaneous identification and detection of 16 anabolic steroid hormones in muscle using liquid chromatography oupled to quadrupole/linear ion trap mass spectrometry]. PG - 991-1001 AB - 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. FAU - Zhang, Hongwei' AU - Zhang H AD - Technical Center of Entry-Exit Inspection and Qurantine, Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266002, China. light04@126.com FAU - Cai, Xue AU - Cai X FAU - Lin, Liming AU - Lin L FAU - Chen, Liangzhen AU - Chen L FAU - Liang, Chengzhu AU - Liang C FAU - Bao, Lei AU - Bao L FAU - Tang, Zhixu AU - Tang Z FAU - Niu, Zengyuan AU - Niu Z FAU - Wang, Fengmei AU - Wang F LA - chi PT - English Abstract PT - Journal Article PT - Research Support, Non-U.S. Gov't PL - China TA - Se Pu JT - Se pu = Chinese journal of chromatography JID - 9424804 RN - 0 (Anabolic Agents) RN - 0 (Androgens) RN - 0 (Gonadal Steroid Hormones) RN - 0 (Progestins) SB - IM MH - Anabolic Agents/analysis MH - Androgens/analysis MH - Animals MH - Chromatography, Liquid/*methods MH - Food Contamination/*analysis MH - Gonadal Steroid Hormones/*analysis MH - Muscle, Skeletal/*chemistry MH - Progestins/analysis MH - Spectrometry, Mass, Electrospray Ionization/*methods EDAT- 2013/02/07 06:00 MHDA- 2014/05/03 06:00 CRDT- 2013/02/07 06:00 PHST- 2013/02/07 06:00 [entrez] PHST- 2013/02/07 06:00 [pubmed] PHST- 2014/05/03 06:00 [medline] AID - 10.3724/sp.j.1123.2012.08017 [doi] PST - ppublish SO - Se Pu. 2012 Oct;30(10):991-1001. doi: 10.3724/sp.j.1123.2012.08017.