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目的建立饮用水中磷酸三(2-氯乙基)酯(TCEP)和磷酸三(2-氯丙基)酯(TCMEP)残留量的固相萃取-气相色谱火焰光度(GC-FPD)测定法。方法采用Oasis HLB固相萃取(SPE)柱对饮用水中有机磷阻燃剂进行提取和富集,采用GCFPD进行测定,HP-5色谱柱(30 m×0.32 mm,0.25μm)。结果 TCEP、TCMEP分别在375~7 500、200~5 000μg/L的线性范围内,所得回归方程均呈较好的线性关系(r>0.998),检出限分别为165、250 ng/L,定量下限分别为550、833 ng/L。该方法对TCEP的回收率为94%~117%,RSD为1.0%~6.5%;对TCEP的回收率为107%~118%,RSD为2.4%~4.5%。结论该方法具有准确度和精密度均较高、重现性好的优点,适合生活饮用水中有机磷阻燃剂TCEP和TCMEP残留的测定。
Objective To establish a gas chromatography-flame photometric (GC-FPD) method for the determination of residual tris (2-chloroethyl) phosphate (TCEP) and tris (2-chloropropyl) phosphate (TCMEP) in drinking water . Methods Oasis HLB solid phase extraction (SPE) column was used to extract and enrich the organophosphorus flame retardants in drinking water and determined by GCFPD. HP-5 column (30 m × 0.32 mm, 0.25 μm) was used. Results The linear regression equations of TCEP and TCMEP in the range of 375-7 500 and 200-5 000 μg / L showed a good linearity (r> 0.998) with detection limits of 165 and 250 ng / L, respectively. The lower limit of quantitation was 550 and 833 ng / L, respectively. The recovery rate of TCEP was 94% ~ 117% and the RSD was 1.0% ~ 6.5%. The recovery of TCEP was 107% ~ 118% with RSD of 2.4% ~ 4.5%. Conclusion The method has the advantages of high accuracy and precision, good reproducibility, and is suitable for the determination of organophosphorus flame retardants TCEP and TCMEP in drinking water.