气相色谱检测冷冻虾仁中邻苯二甲酸酯类增塑剂

Detection Method of PAEs in Frozen Shelled Shrimp by Gas Chromatography

通过对样品前处理和色谱分离条件的研究和优化，建立并验证了冷冻虾仁中17种邻苯二甲酸酯（PAEs）的气相色谱检测方法。采用WelchromP—SCX（60mg／3mL）小柱为样品前处理净化柱。检测条件：石英毛细管柱HP-5（30m×0．25mm，0．25μm）；进样量5μL，不分流；进样口温度250℃；初始温度75℃，以5℃／min升温至300℃，保持10min；检测温度300℃；载气流速1．0mL／min，载气为氮气。PAEs在1-100μg/L范围，线性关系良好，检出限为0．14～0．81μg/L。几种增塑剂的回收率是：DCHP93．20％，DPP81．20％，DMEP78．70％，BMP76．50％，DHXP75．80％，DBP74．70％。冷冻虾仁中含DBP7．77μg/mL，DPP2．36μg/mL，DHXP5．84μg/mL，DINP6．83μg/L，其他增塑剂组分未检出。该方法稳定，结果可靠，重复性好，可用于冷冻虾仁中邻苯二甲酸酯类增塑剂含量的检测。

This study established and tested the method of detection of 17 kinds of PAEs in frozen shelled shrimp by GC. Results showed Welchrom P-SCX 60 mg/3 mL as the clean up column. The experimental conditions： A capillary column HP-5 Column （30 m×0.25 mm, 0.25 μm） ; The injection volume was 5μL; Oven temperature of 75℃, 5 ℃·min-1. The rate rose to 300℃, to maintain 10min; Inlet temperature： 250℃; detector （FID） temperature： 300℃; The begin- ning of the column flow rate of 1.0 mL.min-1; Nitrogen as carrier gas. PAEs in the range of 1-100 μg/mL linear rela- tionship, the detection limit was 0.14--0.81 μg/mL. Recovery rate were DCHP： 93.20%, DPP： 81.20%, DMEP： 78.70%, BMP： 76.50%, DHXP： 75.80%, DBP： 74.70%. Frozen shelled shrimp contained DBP 7.77 μg/mL, DPP 2.36 μg/mL, DHXP 5.84μg/mL, and DINP 6.83 μg/mL. This method is stable, reliable, reproducible, and can be used to detect the content of PAEs in frozen shelled shrimp.