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建立了超声提取法从僵蚕中快速提取草酸铵并采用高效液相色谱紫外检测器进行检测的方法。样品采用50mL超纯水在30℃条件下超声提取10min,以色谱柱Geminu5U C_(18) 110A(250×4.6mm,5μm)进行分离,甲醇/0.5%NH_4H_2PO_4水溶液(10/90,V/V)作为洗脱液,流速为0.4mL/min,最大吸收波长为214nm,外标法定量。在10~200μg/mL范围内线性良好,相关系数R~2=0.9995,样品中分别添加0.05,0.10,0.20g草酸铵,3个添加水平的回收率在101.5%~109.0%,相对标准偏差在0.78%~9.1%之间,方法可用于僵蚕中草酸铵含量的测定。
A rapid extraction method of ammonium oxalate from silkworm silkworm by ultrasonic extraction was established and detected by high performance liquid chromatography with ultraviolet detector. The sample was extracted with 50 mL of ultrapure water under ultrasonic wave at 30 ℃ for 10 min and separated by Geminu5U C_ (18) 110A (250 × 4.6 mm, 5 μm). The methanol / 0.5% NH_4H_2PO_4 aqueous solution (10/90, V / V) As the eluent, the flow rate of 0.4mL / min, the maximum absorption wavelength of 214nm, external standard method. The calibration curve was linear in the range of 10 ~ 200μg / mL with the correlation coefficient of R ~ 2 = 0.9995. The samples were respectively treated with 0.05,0.10,0.20g ammonium oxalate and the recoveries of three added levels were 101.5% -109.0%. The relative standard deviations 0.78% ~ 9.1%, the method can be used for determination of ammonium oxalate in silkworm.