高效液相色谱法测定啶氧菌酯悬浮剂及水分散粒剂中有效成分含量

doi:10.11924/j.issn.1000-6850.casb2021-0125

中国农学通报 ›› 2021, Vol. 37 ›› Issue (27): 117-124.doi: 10.11924/j.issn.1000-6850.casb2021-0125

高效液相色谱法测定啶氧菌酯悬浮剂及水分散粒剂中有效成分含量

马腾飞¹(), 贾孙悦², 刘琳¹, 周芹¹^,³^,⁴(), 高金胜¹()

¹黑龙江大学现代农业与生态环境学院,哈尔滨 150080
²黑龙江大学化学化工与材料学院,哈尔滨 150080
³农业农村部甜菜品质监督检验测试中心,哈尔滨 150080
⁴农业农村部糖料产品质量安全风险评估实验室,哈尔滨 150080

收稿日期:2021-02-03 修回日期:2021-04-13 出版日期:2021-09-25 发布日期:2021-10-28
通讯作者: 周芹,高金胜
作者简介:马腾飞,男,1995年出生,山西太原人,硕士研究生,主要从事农药合成及产品质量检验工作。通信地址：150080 哈尔滨市南岗区学府路74号黑龙江大学农学楼527,Tel：18335442672,E-mail： mtf595180119@163.com。
基金资助:
国家甜菜现代农业产业技术体系项目“质量安全与营养品质评价”(CARS-170503);《农药产品中有效成分测定通用分析方法-液相色谱法》体系建设“啶磺草胺等10个农药品种液相色谱分析方法建立”(14192195)

Active Ingredients in Picoxystrobin Suspension Concentrate and Water Dispersible Granule: Determination by HPLC

Ma Tengfei¹(), Jia Sunyue², Liu Lin¹, Zhou Qin¹^,³^,⁴(), Gao Jinsheng¹()

¹Modern Agriculture and the Ecological Environment Academy of Heilongjiang University, Harbin 150080
²School of Chemistry and Materials Science, Heilongjiang University, Harbin 150080
³Beet Quality Supervision, Inspection and Test Center Ministry of Agriculture and Rural Affairs, Harbin 150080
⁴Laboratory of Quality & Safety Risk Assessment for Sugar Crops Products, Ministry of Agriculture and Rural Affairs, Harbin 150080

Received:2021-02-03 Revised:2021-04-13 Online:2021-09-25 Published:2021-10-28
Contact: Zhou Qin,Gao Jinsheng

摘要/Abstract

摘要：

为了建立在同一液相色谱条件下啶氧菌酯悬浮剂及水分散粒剂中有效成分含量的通用分析方法,样品用乙腈溶解,采用反相高效液相色谱法,流动相为乙腈-水溶液（体积比80:20）,流速1.0 mL/min,进样量5 μL,使用Symmetry-C₁₈色谱柱和二极管阵列检测器,在波长220 nm下对试样中的啶氧菌酯进行高效液相色谱分离,外标法定量。此外,利用二极管阵列检测器进行了峰纯度检验及不同实验室方法验证。结果表明：方法的线性范围在100.1~1000.8 mg/L之间,线性相关系数R²为0.9993;悬浮剂及水分散粒剂的添加回收率平均值分别为100.64%、99.74%,测定结果的相对标准偏差(RSD)值分别为1.31%、0.69%;不同实验室不同仪器之间的重复性标准偏差悬浮剂及水分散粒剂分别为0.8052%、0.6003%,再现性相对标准偏差(RSD_R)分别为0.8560%、1.5625%。方法精密度、准确度及峰纯度结果均符合农药产品分析方法的要求,适用于啶氧菌酯悬浮剂及水分散粒剂中啶氧菌酯含量的测定。

关键词: 啶氧菌酯, 悬浮剂, 水分散粒剂, 高效液相色谱, 有效成分

Abstract:

In order to establish a general method to determine active ingredient in picoxystrobin suspension concentrate (SC) and water dispersible granule (WG) using the same high performance liquid chromatography (HPLC) condition,the samples were dissolved with acetonitrile, and analyzed by RP-HPLC. The mobile phase was acetonitrile-water (volume ratio 80: 20), the flow rate was 1.0 mL/min and the amount of injection was 5.0 μL. Separation was achieved on the Symmetry-C₁₈ column and diode array detector (DAD) at 220 nm, and the quantitative result was calculated by external standard method. In addition, the peak purity was checked through DAD and the method was tested by different laboratories. The result showed good linearities in the concentration ranged from 100.1 mg/L to 1000.8 mg/L, with the correlation coefficient (R²) of 0.9993. The recovery of SC and WG were 100.64% and 99.74%, respectively. The RSD of measurement results were 1.31% and 0.69% respectively. RSD of different laboratories were 0.8052% and 0.6003%. RSD_R were 0.8560% and 1.5625%, respectively. The precision, accuracy and peak purity results meet the requirements of analysis for pesticide products. The method is suitable for the determination active ingredient for picoxystrobin in suspension concentrate and water dispersible granule.

Key words: picoxystrobin, suspension concentrate, water dispersible granule, HPLC, active ingredient

中图分类号:

马腾飞, 贾孙悦, 刘琳, 周芹, 高金胜. 高效液相色谱法测定啶氧菌酯悬浮剂及水分散粒剂中有效成分含量[J]. 中国农学通报, 2021, 37(27): 117-124.

Ma Tengfei, Jia Sunyue, Liu Lin, Zhou Qin, Gao Jinsheng. Active Ingredients in Picoxystrobin Suspension Concentrate and Water Dispersible Granule: Determination by HPLC[J]. Chinese Agricultural Science Bulletin, 2021, 37(27): 117-124.

图/表 11

参考文献 26

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编号	称样质量/g	啶氧菌酯质量分数/%	最大值/%	最小值/%	平均值/%	标准偏差/%	相对标准偏差(RSD)/%
STD-SC-A	0.05127	-	23.08	22.34	22.74	0.29	1.31
SC-A1	0.22201	22.64
SC-A2	0.22202	22.34
SC-A3	0.22298	23.08
SC-A4	0.22219	22.99
SC-A5	0.22278	22.67

编号	称样质量/g	啶氧菌酯质量分数/%	最大值/%	最小值/%	平均值/%	标准偏差/%	相对标准偏差(RSD)/%
STD-SC-A	0.05127	-	23.08	22.34	22.74	0.29	1.31
SC-A1	0.22201	22.64
SC-A2	0.22202	22.34
SC-A3	0.22298	23.08
SC-A4	0.22219	22.99
SC-A5	0.22278	22.67

编号	称样质量/g	啶氧菌酯质量分数/%	最大值/%	最小值/%	平均值/%	标准偏差/%	相对标准偏差(RSD)/%
STD-WG-A	0.05005	-	50.99	50.10	50.53	0.35	0.69
WG-A1	0.09813	50.99
WG-A2	0.09817	50.37
WG-A3	0.09819	50.79
WG-A4	0.09921	50.10
WG-A5	0.09867	50.42

编号	称样质量/g	啶氧菌酯质量分数/%	最大值/%	最小值/%	平均值/%	标准偏差/%	相对标准偏差(RSD)/%
STD-WG-A	0.05005	-	50.99	50.10	50.53	0.35	0.69
WG-A1	0.09813	50.99
WG-A2	0.09817	50.37
WG-A3	0.09819	50.79
WG-A4	0.09921	50.10
WG-A5	0.09867	50.42

溶液名称	试样质量/g	标样质量/g	实测质量/g	回收率/%	平均回收率/%
STD-B	-	0.05005	-	-	100.64
SC-B1	0.11109	0.02519	0.05031	100.73
SC-B2	0.11102	0.02516	0.05041	100.01
SC-B3	0.11124	0.02526	0.04930	98.51
SC-B4	0.11101	0.02501	0.05145	103.47
SC-B5	0.11134	0.02524	0.04984	99.57

高效液相色谱法测定啶氧菌酯悬浮剂及水分散粒剂中有效成分含量

Active Ingredients in Picoxystrobin Suspension Concentrate and Water Dispersible Granule: Determination by HPLC

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参考文献 26

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溶液名称	试样质量/g	标样质量/g	实测质量/g	回收率/%	平均回收率/%
STD-B	-	0.05005	-	-	99.74
WG-B1	0.05074	0.02519	0.05065	100.64
WG-B2	0.05092	0.02534	0.05066	100.18
WG-B3	0.05013	0.02512	0.04923	98.56
WG-B4	0.05023	0.02556	0.05015	99.44
WG-B5	0.05012	0.02514	0.04989	99.85

统计量值	悬浮剂	水分散粒剂
总体平均值Y	22.72	50.18
试验单位数P	4	4
重复性标准偏差S_r	0.1829	0.3012
再现性标准偏差S_R	0.1945	0.7840
重复性r	0.5122	0.8434
再现性R	0.5445	2.1953
重复性相对标准偏差RSD_r	0.8052	0.6003
再现性相对标准偏差RSD_R	0.8560	1.5625
霍维茨值RSD_R (Hor)	2.4998	2.2187

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