目的: 建立超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定蔗糖中47种农药残留量的方法。方法: 蔗糖样品经酸性乙腈提取,氮气吹干浓缩,采用LC-MS/MS 进行分析检测,在多反应检测模式(MRM)下,用空白基质标准曲线-内标法进行定量。结果: 各待测物质在一定浓度范围内线性良好(r>0.995),检测限为0.01~2.00 μg·kg-1。分别在蔗糖样品中添加47 种农药标准溶液10、25、50 μg·kg-1,进行标准添加回收试验,方法回收率为71.0%~106.0%,重复性RSD为0.90%~8.5%。15批蔗糖样品中2批检出噻虫嗪、噻虫胺,其余均未检出。结论: 该方法具有前处理简单快捷、灵敏、准确等优点,符合农药残留检测要求,满足蔗糖中农药残留检测需要,可用于蔗糖的质量控制。
[1] 保国裕, 常国炜, 蓝艳华. 蔗糖的功能性质[J]. 甘蔗糖业, 2023, 52(4):71
BAO GY, CHANG GW, LAN YH. Functional properties of sucrose [J]. Sugar Canes, 2023, 52(4):71
[2] GB 2763-2021食品中农药最大残留限量[S]. 2021
GB 2763-2021 National Food Safety Standard—Maximum Residue Limits for Pesticides in Food[S]. 2021
[3] NY/T 2254-2012甘蔗生产良好农业规范[S]. 2013
NY/T 2254-2012 Good Agricultural Practice for Sugarcn[S]. 2013
[4] 中华人民共和国药典2020 年版.四部[S]. 2020:823,239
ChP 2020. Vol Ⅳ[S]. 2020: 823,239
[5] 王刚, 刘鲁杰, 秦建国, 等.新型分离纯化技术在药用蔗糖制备工艺中的应用[J].化学试剂, 2023, 45(7):10
WANG G, LIU LJ, QIN JG, et al. Application of novel separation and purification technology for the preparation of medicinal sucrose[J]. Chem Reagents, 2023, 45(7):10
[6] 刘刚.我国甘蔗用农药登记及最大残留限量标准制定新进展[J]. 甘蔗糖业, 2021, 50(4):42
LIU G.New progresses in registration and MRL of sugarcane pesticides in China[J]. Sugar Canes, 2021, 50(4):42
[7] 黄惠明, 吴水金, 李跃森, 等.超高效液相色谱串联质谱法检测甘蔗中多种农药残留[J]. 福建分析测试, 2017, 26(4):49
HUANG HM, WU SJ, LI YS, et al. Determination of pesticide residues in sugarcane by ultra-performance liquid chromatography tandem mass spectrometry[J]. Fujian Anal Test, 2017, 26(4):49
[8] 曾秋霞, 黄敏兴, 郑冰仪, 等.气相色谱-串联三重四极杆质谱法测定甘蔗中苯酰胺类农药残留[J]. 甘蔗糖业, 2022, 51(3):44
ZENG QX, HUANG MX, ZHENG BY, et al. Determination of benzamide pesticide residues in sugarcane by gas chromatography-tandem triple quadrupole mass spectrometry [J]. Sugar Canes, 2022, 51(3):44
[9] 李长成, 黄敏兴, 陈其钊, 等. QuEChERs-超高效液相色谱-串联质谱检测甘蔗中15 种有机磷农药残留量的方法研究[J]. 甘蔗糖业, 2021, 50(6):25
LI CC, HUANG MX, CHEN QZ, et al. The determination of 15 organic phosphorus pesticide pesidues in sugarcane by QuEChERs-UPLC-MS/MS[J]. Sugar Canes, 2021, 50(6):25
[10] 高裕锋, 甄振鹏, 郭剑雄, 等. 高效液相色谱串联质谱测定甘蔗中12 种氨基甲酸酯类农药残留[J]. 甘蔗糖业, 2013, (1):58
GAO YF, ZHEN ZP, GUO JX, et al. Determination of 12 carbamate pesticide residues in sugarcane by HPLC-MS/MS[J]. Sugar Canes, 2013, (1):58
[11] BOZENA L, GULZHAKHAN I, PIOTR K, et al. Multi-residue methods for the determination of over four hundred pesticides in solid and liquid high sucrose content matrices by tandem mass spectrometry coupled with gas and liquid chromatograph[J]. Talanta, 2016,151:51
[12] 刘芫汐, 左甜甜, 王莹, 等. 山楂叶中127 种农药多残留检测分析[J]. 药物分析杂志, 2022, 42(9):1586
LIU YX, ZUO TT, WANG Y, et al. Determination and analysis of 127 pesticide residues in hawthorn leaves[J]. Chin J Pharm Anal, 2022, 42(9):1586
[13] 王成龙, 刘佳, 徐振林, 等. 超高效液相色谱- 串联质谱法检测6 种样品基质中百草枯农药残留[J]. 药物分析杂志, 2022, 42(12):2155
WANG CL, LIU J, XU ZL, et al.Determination of paraquat residues in 6 sample matrices by ultra performance liquid chromatograph-tandem mass spectrometry [J]. Chin J Pharm Anal, 2022, 42(12):2155
[14] 李道霞, 周佳, 姚欢, 等. dMRM模式下的高效液相色谱串联质谱法同时检测蔬菜中327种农药残留[J]. 中国果菜, 2022, 42(6):36
LI DX, ZHOU J, YAO H, et al. Determination of 327 pesticide residues in vegetables by HPLC-MS/MS with dynamic multi-reaction monitoring [J]. China Fruit Veget, 2022, 42(6):36
[15] 高娜, 乔颖, 刘雪红, 等. Sin-QuEChERS-GC-MS/MS 法快速测定人参中47 种残留农药[J]. 药物分析杂志, 2022, 42(12):2145
GAO N, QIAO Y, LIU XH, et al. Rapid determination of 47 kinds of pesticide residues in Ginseng Radix et Rhizoma by Sin-QuEChERS-GC-MS/MS[J]. Chin J Pharm Anal, 2022, 42(12):2145
[16] 闫琪颖, 王晓蕾, 苏建, 等. 基于多元统计学的北沙参主产地农药残留状况分析[J]. 药物分析杂志, 2023, 43(4):644
YAN QY, WANG XL, SU J, et al. Analysis of pesticide residues in Radix Glehniae from main habitats based on the multivariate statistics analysis[J]. Chin J Pharm Anal, 2023, 43(4):644
[17] GB 23200.8-2016食品安全国家标准水果和蔬菜中500种农药及相关化学品残留量的测定气相色谱-质谱法[S]. 2017
GB 23200.8-2016 National food Safety Standards-Determination of 500 Pesticides and Related Chemicals Residues in Fruits and Vegetables Gas Chromatography-Mass Spectrometry[S]. 2017
[18] GB 23200.13-2016食品安全国家标准茶叶中448种农药及相关化学品残留量的测定液相色谱-质谱法 [S]. 2017
GB 23200.13-2016 National Food Safety Standards-Determination of 448 Pesticides Residues in Tea Liquid Chromatography-Mass Spectrometry[S]. 2017
[19] 平文卉, 史玉坤, 杨清华, 等. 高效液相色谱-串联质谱法测定药食同源中药材中29种农药残留[J]. 化学分析计量, 2023, 32(11):47
PING WH, SHI YK, YANG QH, et al. Determination of 29 pesticide residues in medicinal and edible traditional chinese medicine by high performance liquid chromatography-tandem mass spectrometry [J]. Chem Anal Meterag, 2023, 32(11):47
[20] 章会琼, 杨琴, 蒲雪, 等. 高效液相色谱串联质谱法快速检测淫羊藿药材中47种农药残留[J]. 中国药业, 2023, 32(22):103
ZHANG HQ, YANG Q, PU X, et al. Rapid detection of 47 pesticide residues in Epimedii Folium by HPLC - MS/MS [J]. China Pharm, 2023, 32(22):103
