A method for the analysis of five types of triphenylmethane dye residues in water was developed by using solid phase extraction ( SPE) combined with ultra performance liquid chromatography coupled to triple quadrupole linear ion trap mass spectrometry ( UPLC-MS/MS/MS ) . The water samples were extracted and cleaned with mixed-mode cation exchange solid-phase extraction cartridges ( MCX) . The UPLC separation was performed on a C18 column with a linear gradient elution program of acetonitrile and 5 mmol/L aqueous ammonium acetate ( containing 0. 02% formic acid) as mobile phase. Triphenylmethane dye residues were analyzed by mass spectrometry under an electrospray ionization interface ( ESI ) in positive ion mode with MRM-IDA-EPI mode. The calibration curves of five types of triphenylmethane dyes were linear in the range of 0. 02-20 μg/L, and the correlation coefficients were not less than 0. 998. The recoveries at spiked levels of 5 , 10 and 20 μg/L were in the range of 70 . 9%-101%, and the RSDs were 3 . 4%-11 . 9% ( n=6 ) . The limit of detection and quantification were 0. 42-2. 18 ng/L and 1. 68-8. 73 ng/L, respectively. The method was performed as sensitive and accurate, and also suitable for simultaneous determination of five types of triphenylmethane dye residues in water.%建立了固相萃取( SPE)/超高效液相色谱-三重四极杆/复合线性离子阱质谱( UPLC-MS/MS/MS)同时测定水体中孔雀石绿(MG)、结晶紫(CV)、亮绿(BG)及其代谢产物隐性孔雀石绿(LMG)和隐性结晶紫(LCV)5种三苯甲烷类残留的方法。100 mL水样过滤后用对甲苯磺酸溶液调节pH=4,经MCX阳离子固相萃取柱富集净化后,采用BEH C18色谱柱,以乙腈-5 mmol/L乙酸铵溶液(含0.02%甲酸)作为流动相进行梯度洗脱,采用“杆-阱扫描”( MRM-IDA-EPI)正离子模式进行检测。5种三苯甲烷类物质MG, LCV, BG, LMG和CV在0.02~10μg/L浓度范围内线性良好(r>0.998),回收率为70.9%~101%,相对标准偏差(RSD, n=6)为3.4%~11.9%,方法检出限为0.42~2.2 ng/L,定量限为1.7~8.7 ng/L。本方法快速、灵敏,适用于水体中5种三苯甲烷类残留物的痕量测定。
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