高效液相色谱-质谱联用法对线性烷基苯磺酸钠同系物的检测

Determination of Sodium Alkylbenzene Sulfonates by High Performance Liquid Chromatography and Electrospray Ionization Mass Spectroscopy

首次利用高效液相色谱-质谱联用技术,建立了纺织品中线性烷基苯磺酸钠（LAS）同系物的检测方法。采用甲醇超声提取法进行前处理,并优化了超声提取的温度、时间和提取试剂用量。以C18反相柱为分析柱,甲醇、醋酸铵为流动相,在10 min内完成对LAS的定性、定量分析。LAS质谱检测的母离子为m/z297.0、311.0、325.0、339.0、352.9,定量子离子为m/z182.8。LAS检测的线性范围为10-1 000μg/kg,相关系数不小于0.999,检出限为2.0μg/kg。LAS的回收率为92%-100%,相对标准偏差不大于12.5%。

A high performance liquid chromatography and electrospray ionization mass spectroscopy （HPLC -ESI MS） method was developed for determination of alkylbenzene sulfonates （LAS）. LAS in fabric were extracted by methanol with ultrasonic wave. The extract was separated on a C 18 reversed phase column with methanol and 5 mmol/L ammonium acetate as the mobile phase at the flow rate of 0. 3 mL/min, and determined by ESI MS/MS. The parent ions of LAS were m/z 297. 0, 311.0, 325.0, 339. 0, 352. 9, and the daughter ion of m/z 182. 8 was selected as quantitative ion. The experimental conditions such as extraction temperature, time and volume of reagent were optimized. Under the optimal conditions, linear range of the calibration curves for LAS was in the range of 10 - 1 000 μg/kg with correlation coefficient no less than 0. 999. The limit of detection （ S/N ≥ 3 ） was 2. 0 μg/kg. The recoveries were in the range of 92% - 100% with RSDs no more than 12. 5%.