| 高效阴离子交换-积分脉冲法检测氨基寡糖素农药中游离氨基葡萄糖 |
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| 引用本文： | 陈炜瑶,吴国权,李彬,高凡钦.高效阴离子交换-积分脉冲法检测氨基寡糖素农药中游离氨基葡萄糖[J].农药学学报,2022,24(3):655-658. |
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| 作者姓名： | 陈炜瑶 吴国权 李彬 高凡钦 |
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| 作者单位： | 1.广西中医药大学，南宁 530000 |
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| 摘 要： | 建立了采用高效阴离子交换-积分脉冲法检测氨基寡糖素母药及水剂中游离氨基葡萄糖含量的方法。以DionexAminoTrap Column (氨基捕获柱)和DionexCarboPac PA100阴离子交换柱为分离柱，用17 mmol/L的氢氧化钠溶液洗脱目标物游离氨基葡萄糖，200 mmol/L的氢氧化钠溶液冲洗氨基寡糖素，流速为1.0 mL/min，总分析时间为30 min。在最优分离条件下，可消除氨基寡糖素对氨基葡萄糖的干扰，氨基葡萄糖的检出限可达到0.01 mg/L (S/N=3)，标准线性范围为0.02~10 mg/L，相关系数为0.9999。对市售的氨基寡糖素母药及水剂进行检测，3次平行样品相对标准偏差小于1.9%，添加回收率在90%~99%之间，检测结果准确可靠。该方法可用于氨基寡糖素母药及水剂中游离氨基葡萄糖的检测，对氨基寡糖素农药质量判断具有一定指导意义。
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| 关 键 词： | 阴离子交换-积分脉冲 氨基寡糖素 氨基葡萄糖 离子色谱 壳寡糖 |
| 收稿时间： | 2021-07-14 |
High?performance?anion?exchange-integral?pulse method for detection of free glucosamine in amino-oligosaccharins pesticides |
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| Institution: | 1.Guangxi University of Chinese Medicine, Nanning 530000, China2.Wuzhou Institute for Food and Drug Control, Wuzhou 543000, Guangxi Zhuang Autonomous Region, China3.Thermo Fisher Scientific (China) Co., Ltd., Shanghai 200135, China |
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| Abstract: | A high performance anion exchange-integral pulse method was established to determine the content of free glucosamine in amino-oligosaccharin technical concentrates and aqueous solution. Using the DionexAminoTrap Column and DionexCarboPac PA100 anion exchange column as the separation column, the target free glucosamine was eluted with 17 mmol/L sodium hydroxide, and the chitosan oligosaccharide was flushed by 200 mmol/L sodium hydroxide. The flow rate was 1.0 mL/min, and the total analysis time was 30 min. Under the optimal separation conditions, the interference of chitosan oligosaccharides on glucosamine could be eliminated. The detection limits of glucosamine reached 0.01 mg/L (S/N=3), the calibration curve ranged from 0.02 to 10 mg/L, and the correlation coefficients was 0.999 9. For the analysis of commercially available amino-oligosaccharin technical concentrates and aqueous solution at 3 replicates, the relative standard deviation was less than 1.9%, and the spiked recoveries were between 90%-99%, which indicated that the established method was accurate and reliable. Therefore, this method could be used for the detection of free glucosamine in amino-oligosaccharin technical concentrates and aqueous solution, and could provide method for the quality evaluation of the amino-oligosaccharin pesticides. |
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