title: Sensitive determination of cholesterol and its metabolic steroid hormones by UHPLC-MS/MS via derivatization coupled with dual ultrasonic-assisted dispersive liquid-liquid microextraction.
abstract: Quantitative analysis of cholesterol and its metabolic steroid hormones plays a vital role in diagnosing endocrine disorders and understanding disease progression, as well as in clinical medicine studies. Because of their extremely low abundance in body fluids, it remains a challenging task to develop a sensitive detection method.
  
  
  
  A hyphenated technique of dual ultrasonic-assisted dispersive liquid-liquid microextraction (dual-UADLLME) coupled with microwave-assisted derivatization (MAD) was proposed for cleansing, enrichment and sensitivity enhancement. 4'-Carboxy-substituted rosamine (CSR) was synthesized and used as derivatization reagent. An ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method was developed for determination of cholesterol and its metabolic steroid hormones in the multiple reaction monitoring mode.
  
  
  
  Parameters of dual-UADLLME, MAD and UHPLC-MS/MS were all optimized. Satisfactory linearity, recovery, repeatability, accuracy and precision, absence of matrix effect and extremely low limits of detection (LODs, 0.08-0.15 pg mL(-1) ) were achieved.
  
  
  
  Through the combination of dual-UADLLME and MAD, a determination method for cholesterol and its metabolic steroid hormones in human plasma, serum and urine samples was developed and validated with high sensitivity, selectivity, accuracy and perfect matrix effect results. Copyright © 2016 John Wiley & Sons, Ltd.
authors.affiliation: Shandong Provincial Key Laboratory of Life-Organic Analysis and Key Laboratory of Pharmaceutical Intermediates and Analysis of Natural Medicine, College of Chemistry and Chemical Engineering, Qufu Normal University, Qufu, 273165, Shandong, China.|Beijing National Laboratory for Molecular Sciences, Key Laboratory of Bioorganic Chemistry and Molecular Engineering of Ministry of Education, Institute of Analytical Chemistry, College of Chemistry and Molecular Engineering, Peking University, Beijing, 100871, China.
authors.forename: Xian-En
authors.initials: XE
authors.lastname: Zhao
authors.affiliation: Shandong Provincial Key Laboratory of Life-Organic Analysis and Key Laboratory of Pharmaceutical Intermediates and Analysis of Natural Medicine, College of Chemistry and Chemical Engineering, Qufu Normal University, Qufu, 273165, Shandong, China.|Hospital of University, Qufu Normal University, Qufu, 273165, Shandong, China.
authors.forename: Ping
authors.initials: P
authors.lastname: Yan
authors.affiliation: Shandong Provincial Key Laboratory of Life-Organic Analysis and Key Laboratory of Pharmaceutical Intermediates and Analysis of Natural Medicine, College of Chemistry and Chemical Engineering, Qufu Normal University, Qufu, 273165, Shandong, China.|College of Life Science, Qufu Normal University, Qufu, 273165, Shandong, China.
authors.forename: Renjun
authors.initials: R
authors.lastname: Wang
authors.affiliation: Shandong Provincial Key Laboratory of Life-Organic Analysis and Key Laboratory of Pharmaceutical Intermediates and Analysis of Natural Medicine, College of Chemistry and Chemical Engineering, Qufu Normal University, Qufu, 273165, Shandong, China.
authors.forename: Shuyun
authors.initials: S
authors.lastname: Zhu
authors.affiliation: Shandong Provincial Key Laboratory of Life-Organic Analysis and Key Laboratory of Pharmaceutical Intermediates and Analysis of Natural Medicine, College of Chemistry and Chemical Engineering, Qufu Normal University, Qufu, 273165, Shandong, China.
authors.forename: Jinmao
authors.initials: J
authors.lastname: You
authors.affiliation: Beijing National Laboratory for Molecular Sciences, Key Laboratory of Bioorganic Chemistry and Molecular Engineering of Ministry of Education, Institute of Analytical Chemistry, College of Chemistry and Molecular Engineering, Peking University, Beijing, 100871, China.
authors.forename: Yu
authors.initials: Y
authors.lastname: Bai
authors.affiliation: Beijing National Laboratory for Molecular Sciences, Key Laboratory of Bioorganic Chemistry and Molecular Engineering of Ministry of Education, Institute of Analytical Chemistry, College of Chemistry and Molecular Engineering, Peking University, Beijing, 100871, China.
authors.forename: Huwei
authors.initials: H
authors.lastname: Liu
mesh_terms: D002784:Cholesterol / Q000032:analysis* / Q000097:blood / Q000652:urine; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005260:Female; D006728:Hormones / Q000032:analysis* / Q000097:blood / Q000652:urine; D006801:Humans; D057230:Limit of Detection; D059627:Liquid Phase Microextraction / Q000295:instrumentation / Q000379:methods*; D008297:Male; D008872:Microwaves; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013256:Steroids / Q000032:analysis / Q000097:blood / Q000652:urine; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014465:Ultrasonics
chemical_list: D006728:Hormones; D013256:Steroids; D002784:Cholesterol