Quantitative Analysis of Chloramphenicol in Royal Jelly by Column-switching LC-MS/MS Using a Pretreatment Column with a Higher-pressure Capability

• Published in: Analytical Sciences 2015/05/10, Vol.31(5), pp.445-450
• Main Authors: KAWANO, Shin-ichi, HAYAKAWA, Yoshihiro, HASHI, Yuki, LIN, Jin-Ming
• Format: Article
• Language: English
• Subjects: Analytical Chemistry; Chemistry; Chloramphenicol; Chloramphenicol - analysis; Chromatography, High Pressure Liquid; Dynamical systems; Dynamics; Fatty Acids - chemistry; LC-MS/MS; Liquids; Mathematical analysis; methylcellulose; on-line pretreatment; On-line systems; Pressure; Pretreatment; Quantitative analysis; Regulations; restricted access media; royal jelly; Tandem Mass Spectrometry
• ISSN: 0910-6340; 1348-2246
• DOI: 10.2116/analsci.31.445

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.