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High Sensitive Analysis of Bromate by LC/MS/MS (JJ-50 2D)

The standard value of bromate in Japan is set to 0.01mg/L by Ministry of Health, Labour and Welfare. Although the current analysis of bromate adopts ion chromatography with post column-adsorption photometry, liquid chromatography with mass spectrometry was added by the Ministry of Health, Labor and Welfare on April 1, 2017. In this application, RSpak JJ-50 2D was used for an LC/MS/MS analysis of bromate. JJ-50 is modified with quaternary ammonium functional group and it works as a multimode column (reversed phase + anion exchange). Bromate can be separated from other major anions, and the calibration curve of bromate shows good linearity respectively in the range from 0.001 to 0.02mg/L. Furthermore, when 0.01mg/L of bromate was added to tap water, additional recovery of bromate was almost 100%.


Sample : 5μL
Standard solution
1. ClO3, Chlorate 0.01mg/L
2. NO3, Nitrate 0.1mg/L
3. BrO3, Bromate 0.01mg/L
4. Br, Bromide 0.1mg/L
5. Cl, Chloride 0.1mg/L
6. SO42-, Sulfate 0.1mg/L

Sample : 5μL
Tap water
1. ClO3, Chlorate
2. NO3, Nitrate
3. BrO3, Bromate
4. Br, Bromide
5. Cl, Chloride
6. SO42-, Sulfate








Column       : Shodex RSpak JJ-50 2D (2.0mmI.D. x 150mm)
Eluent       : (A); 200mM HCOONH4 aq./(B); CH3CN
               Linear gradient (High pressure);
               B%; 85% (0min) → 85% (8min) → 50% (9min) → 50% (14min) 
                   → 85% (15min) → 85% (20min)
Flow rate    : 0.3mL/min
Detector     : ESI-MS/MS (MRM Negative) for ClO3-, BrO3-
               ESI-MS (SIM Negative) for NO3-, Br-, Cl-, SO42-
Column temp. : 50°C