LC/MS/MS Analysis of Bromate According to Japanese Water Supply Act (JJ-50 2D)

Under the Ordinance on Water Quality Standards (MHLW Ministerial Ordinance No. 101, May 30, 2003), the standard value for bromate is set at ≤ 0.01 mg/L. In addition, the official methods in “Methods Prescribed by the Minister of Health, Labour and Welfare Based on the Provisions of the Ordinance on Water Quality Standards” (MHLW Notification No. 261, July 22, 2003; last amended by Notification No. 87*, March 28, 2017) include “Table 18: Ion Chromatography–Post-Column Absorptiometry Method”, and “Table 18-2: Liquid Chromatography–Mass Spectrometry (LC–MS/MS)” newly added bromate analysis. This method mentions using a column packed with silica or polymer-based gels modified with anion‑exchange group, or a column offering equivalent or superior separation performance. Using RSpak JJ-50 2D, a multimode (reversed phase and anion exchange modes) column modified with quaternary ammonium group, we analyzed standard solutions of halogen oxides and common anions, as well as tap water. Under the described conditions, bromate was resolved from other major anions. The calibration curve for bromate showed high linearity over 0.001 to 0.02 mg/L. When tap water was spiked with bromate at 0.01 mg/L, the recovery was approximately 100%.
**Target analyte in Table 18-2 includes bromate.
Refer to "LC/MS/MS Analysis of Chlorate and Bromate According to Japanese Water Supply Act (JJ-50 2D)".

(Note)
As of April 1, 2024, responsibility for water quality measures (such as establishing water quality standards and determining methods for water quality inspections conducted by water utilities) has been transferred from the Ministry of Health, Labour and Welfare to the Ministry of the Environment. Consequently, the name has been changed to “Methods Prescribed by the Minister of the Environment Based on the Provisions of the Ordinance on Water Quality Standards”.

*The version at the time of the application acquisition.

Sample: 5 µL
Standard solution

  1. 1.ClO3-, Chlorate 0.01 mg/L
  2. 2.NO3-, Nitrate 0.1 mg/L
  3. 3.BrO3-, Bromate 0.01 mg/L
  4. 4.Br-, Bromide 0.1 mg/L
  5. 5.Cl-, Chloride 0.1 mg/L
  6. 6.HSO4-, Hydrogen sulfate 0.1 mg/L

Sample: 5 µL
Tap water

  1. 1.ClO3-, Chlorate
  2. 2.NO3-, Nitrate
  3. 3.BrO3-, Bromate
  4. 4.Br-, Bromide
  5. 5.Cl-, Chloride
  6. 6.HSO4-, Hydrogen sulfate
Column
Shodex RSpak JJ-50 2D (2.0 mm I.D. x 150 mm)
Eluent
(A); 200 mM HCOONH4 aq./(B); CH3CN
Linear gradient (High pressure); 85 B % (0 min) → 85 B % (8 min) → 50 B % (9 min) → 50 B % (14 min) → 85 B % (15 min) → 85 B % (20 min)
Flow rate
0.3 mL/min
Detector
ESI-MS/MS (MRM Negative) for ClO3-, BrO3-
ESI-MS (SIM Negative) for NO3-, Br-, Cl-, HSO4-
Column temp.
50 ℃

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