title: Quantitative Analysis of Chloramphenicol in Royal Jelly by Column-switching LC-MS/MS Using a Pretreatment Column with a Higher-pressure Capability.
abstract: An on-line pretreatment liquid chromatography-tandem mass spectrometry (LC-MS/MS) system was developed for the analysis of chloramphenicol (CAP) in royal jelly. A novel methylcellulose-immobilized restricted access media column with a higher-pressure capability of 60 MPa (MC-ODS HP) was developed for the effective removal of proteins and other compounds in the sample matrix. CAP in a sample solution was extracted in 2 min by the column-switching LC-MS/MS system. The system provides a minimum sample pretreatment along with highly sensitive and reproducible analysis. As a result, the limit of quantitation of CAP was 10 pg/mL (= 0.1 μg/kg royal jelly) and the linear dynamic range was between 10 and 10000 pg/mL (correlation coefficient greater than 0.999). The proposed method meets the requirements of regulations in EU (0.3 μg/kg). The inter-day precision and accuracy of CAP at 100 pg/mL over 3 days were 4.5 and 95.4%, respectively. Compared with the conventional method with a pressure of below 25 MPa, the peak separation in the MRM chromatogram was improved by using smaller particles (1.6 μm) for the analytical ODS column. The LC-MS/MS system with an MC-ODS HP expanded the applicability of the automated pretreatment.
authors.affiliation: Shimadzu Global COE for Application & Technical Development, Shimadzu (China) Co., Ltd.
authors.forename: Shin-ichi
authors.initials: S
authors.lastname: Kawano
authors.forename: Yoshihiro
authors.initials: Y
authors.lastname: Hayakawa
authors.forename: Yuki
authors.initials: Y
authors.lastname: Hashi
authors.forename: Jin-Ming
authors.initials: JM
authors.lastname: Lin
mesh_terms: D002701:Chloramphenicol / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid; D005227:Fatty Acids / Q000737:chemistry*; D011312:Pressure; D053719:Tandem Mass Spectrometry; D000099219:Royal Jelly
chemical_list: D002701:Chloramphenicol; D005227:Fatty Acids; D000099219:Royal Jelly