快速阳极化不锈钢丝固相微萃取-高效液相色谱法测定水中苯并[a]芘含量

HPLC Determination of Benzo[a]pyrene in Water with Rapid Anodization of Stainless Steel Wire as Solid-Phase Microextraction Fiber

采用快速阳极氧化不锈钢丝作为固相微萃取纤维-高效液相色谱法测定水中苯并[a]芘的含量。结果表明：阳极氧化不锈钢丝制作简单、稳定性好、寿命长。水样用固相微萃取头在30℃和1000r·min-1搅拌速率下萃取40min，萃取头解吸3min。以C18反相色谱柱为分离柱，以甲醇-水（95＋5）混合液为流动相进行色谱分离。在检测波长254nm处进行测定。苯并[a]芘的质量浓度在0．1～100μg·L叫范围内与其峰面积呈线性关系，检出限（3s／N）为10．92ng·L-1在10，50肚g·L叫等2个浓度水平进行加标回收试验，回收率在97．9％～110％之间。

Stainless steel wire was rapidly anodized and use as extraction fiber in SPME separation which was combined with the HPLC determination of benzo[a]pyrene in water. It was found that the anodized stainless steel wire was easy to prepare, chemically and mechanically stable and durable. The water sample was extracted with the SPME fibrous head for 40 min at 30℃ with stirring at the rate of 1 000 r · min-1. The microextraction head was desorbed for 3 min. C18 reverse phase chromatographic column was used as stationary phase, and methanol-H20 （95-4-5） mixture was used as mobile phase in the chromatographic separation. UV-detection at 254 nm was adopted in the determination. Linear relationship between values of peak area and mass concentration of benzo[-a]pyrene was kept in the range of 0. 1--100μg · L-1 , with detection limit （3S/N） of 10. 92 ng ·L-1. Tests for recovery were made by standard addition method at the concentration levels of 10 μg · L-1 and 50 μg ·L-1 , giving values of recovery in the ranges of 97.9%--110%.