Journal of Zhejiang Agricultural Sciences ›› 2023, Vol. 64 ›› Issue (4): 921-926.DOI: 10.16178/j.issn.0528-9017.20220637
Previous Articles Next Articles
Received:2022-06-07
Online:2023-04-11
Published:2023-03-29
CLC Number:
Add to citation manager EndNote|Ris|BibTeX
URL: http://www.zjnykx.cn/EN/10.16178/j.issn.0528-9017.20220637
| 化合物 | 分子式 | 分子量 | 母离子/ (m/z) | 子离子/ (m/z) | 锥孔电压/ V | 碰撞能量/ V | 定性/ 定量 |
|---|---|---|---|---|---|---|---|
| 抑霉唑 | C14H14Cl2N2O | 297.2 | 297.1 | 159 | 30 | 30 | 定量 |
| 69 | 30 | 25 | 定性 |
| 化合物 | 分子式 | 分子量 | 母离子/ (m/z) | 子离子/ (m/z) | 锥孔电压/ V | 碰撞能量/ V | 定性/ 定量 |
|---|---|---|---|---|---|---|---|
| 抑霉唑 | C14H14Cl2N2O | 297.2 | 297.1 | 159 | 30 | 30 | 定量 |
| 69 | 30 | 25 | 定性 |
| 流动相比例A/B | k'1 | k'2 | α | RS |
|---|---|---|---|---|
| 5/95 | 0.82 | 0.99 | 0.83 | 1.58 |
| 15/85 | 0.90 | 1.09 | 0.84 | 1.83 |
| 25/75 | 1.01 | 1.19 | 0.85 | 2.21 |
| 35/65 | 1.77 | 2.07 | 0.86 | 2.63 |
| 流动相比例A/B | k'1 | k'2 | α | RS |
|---|---|---|---|---|
| 5/95 | 0.82 | 0.99 | 0.83 | 1.58 |
| 15/85 | 0.90 | 1.09 | 0.84 | 1.83 |
| 25/75 | 1.01 | 1.19 | 0.85 | 2.21 |
| 35/65 | 1.77 | 2.07 | 0.86 | 2.63 |
| 流速/(mL·min-1) | k'1 | k'2 | α | RS |
|---|---|---|---|---|
| 0.3 | 0.87 | 1.01 | 0.86 | 1.86 |
| 0.4 | 0.67 | 0.78 | 0.85 | 1.67 |
| 0.5 | 0.69 | 0.78 | 0.85 | 1.83 |
| 0.6 | 0.71 | 0.83 | 0.85 | 1.50 |
| 流速/(mL·min-1) | k'1 | k'2 | α | RS |
|---|---|---|---|---|
| 0.3 | 0.87 | 1.01 | 0.86 | 1.86 |
| 0.4 | 0.67 | 0.78 | 0.85 | 1.67 |
| 0.5 | 0.69 | 0.78 | 0.85 | 1.83 |
| 0.6 | 0.71 | 0.83 | 0.85 | 1.50 |
| 化合物 | 基质 | 回归方程 | 决定系数R2 | 线性范围/(μg·L-1) | 基质效应/% | 定量限/(μg·kg-1) |
|---|---|---|---|---|---|---|
| (S)-(+)-抑霉唑 | 乙腈 | y=1 002.3x-31 100 | 0.995 0 | 2.5~100 0 | ||
| 草莓 | y=365x-828.62 | 0.999 9 | 2.5~100 0 | -63.5 | 5 | |
| (R)-(-)-抑霉唑 | 乙腈 | y=483.7x-11 377 | 0.995 8 | 2.5~100 0 | ||
| 草莓 | y=336.63x+8 322.6 | 0.999 3 | 2.5~100 0 | -30.4 | 5 |
| 化合物 | 基质 | 回归方程 | 决定系数R2 | 线性范围/(μg·L-1) | 基质效应/% | 定量限/(μg·kg-1) |
|---|---|---|---|---|---|---|
| (S)-(+)-抑霉唑 | 乙腈 | y=1 002.3x-31 100 | 0.995 0 | 2.5~100 0 | ||
| 草莓 | y=365x-828.62 | 0.999 9 | 2.5~100 0 | -63.5 | 5 | |
| (R)-(-)-抑霉唑 | 乙腈 | y=483.7x-11 377 | 0.995 8 | 2.5~100 0 | ||
| 草莓 | y=336.63x+8 322.6 | 0.999 3 | 2.5~100 0 | -30.4 | 5 |
| 化合物 | 添加水平/ (μg·kg-1) | 日间(n=6) | 日内(n=16) RSD/% | |||||
|---|---|---|---|---|---|---|---|---|
| 1 d | 2 d | 3 d | ||||||
| 回收率/% | RSD/% | 回收率/% | RSD/% | 回收率/% | RSD/% | |||
| (S)-(+)-抑霉唑 | 5 | 105.9 | 0.5 | 108.5 | 2.2 | 105.2 | 3.4 | 2.0 |
| 50 | 94.6 | 4.4 | 119.7 | 7.1 | 110.4 | 5.2 | 5.6 | |
| 1 000 | 99.2 | 9.5 | 112.9 | 9.0 | 104.3 | 6.4 | 8.3 | |
| (R)-(-)-抑霉唑 | 5 | 97.0 | 5.0 | 117.3 | 5.3 | 101.2 | 4.7 | 5.0 |
| 50 | 89.8 | 9.5 | 113.6 | 11.3 | 99.4 | 7.9 | 9.6 | |
| 1 000 | 86.6 | 8.1 | 110.3 | 4.5 | 105.3 | 5.5 | 6.0 | |
| 化合物 | 添加水平/ (μg·kg-1) | 日间(n=6) | 日内(n=16) RSD/% | |||||
|---|---|---|---|---|---|---|---|---|
| 1 d | 2 d | 3 d | ||||||
| 回收率/% | RSD/% | 回收率/% | RSD/% | 回收率/% | RSD/% | |||
| (S)-(+)-抑霉唑 | 5 | 105.9 | 0.5 | 108.5 | 2.2 | 105.2 | 3.4 | 2.0 |
| 50 | 94.6 | 4.4 | 119.7 | 7.1 | 110.4 | 5.2 | 5.6 | |
| 1 000 | 99.2 | 9.5 | 112.9 | 9.0 | 104.3 | 6.4 | 8.3 | |
| (R)-(-)-抑霉唑 | 5 | 97.0 | 5.0 | 117.3 | 5.3 | 101.2 | 4.7 | 5.0 |
| 50 | 89.8 | 9.5 | 113.6 | 11.3 | 99.4 | 7.9 | 9.6 | |
| 1 000 | 86.6 | 8.1 | 110.3 | 4.5 | 105.3 | 5.5 | 6.0 | |
| 时间/ d | 平均浓度±标准偏差/(μg·kg-1) | EF | |
|---|---|---|---|
| (S)-(+)-抑霉唑 | (R)-(-)-抑霉唑 | ||
| 0.083 | 666.24±3.00 | 649.46±7.91 | 0.51±0.002 |
| 1 | 639.48±19.91 | 645.19±15.44 | 0.50±0.001 |
| 2 | 527.85±16.00 | 560.77±9.60 | 0.49±0.004 |
| 3 | 410.35±21.82 | 451.05±16.61 | 0.48±0.002 |
| 5 | 292.13±31.31 | 337.90±10.31 | 0.45±0.003 |
| 7 | 232.37±33.55 | 268.64±22.78 | 0.45±0.005 |
| 14 | 93.02±12.87 | 124.54±12.56 | 0.43±0.009 |
| 21 | 50.40±0.93 | 66.11±3.62 | 0.43±0.011 |
| 27 | 49.26±11.21 | 58.23±1.21 | 0.42±0.013 |
| 时间/ d | 平均浓度±标准偏差/(μg·kg-1) | EF | |
|---|---|---|---|
| (S)-(+)-抑霉唑 | (R)-(-)-抑霉唑 | ||
| 0.083 | 666.24±3.00 | 649.46±7.91 | 0.51±0.002 |
| 1 | 639.48±19.91 | 645.19±15.44 | 0.50±0.001 |
| 2 | 527.85±16.00 | 560.77±9.60 | 0.49±0.004 |
| 3 | 410.35±21.82 | 451.05±16.61 | 0.48±0.002 |
| 5 | 292.13±31.31 | 337.90±10.31 | 0.45±0.003 |
| 7 | 232.37±33.55 | 268.64±22.78 | 0.45±0.005 |
| 14 | 93.02±12.87 | 124.54±12.56 | 0.43±0.009 |
| 21 | 50.40±0.93 | 66.11±3.62 | 0.43±0.011 |
| 27 | 49.26±11.21 | 58.23±1.21 | 0.42±0.013 |
| [1] | 班思凡, 李春梅, 贺青华, 等. 设施栽培草莓中农药残留膳食风险评估[J]. 食品工业科技, 2020, 41(3): 212-220. |
| [2] | 付岩, 张亮, 吴银良. 草莓中嘧霉胺的残留与膳食风险评估[J]. 现代食品科技, 2017, 33(11): 206-211. |
| [3] | 陈宗懋. 食品中农药残留检测发展的新趋势[J]. 农产品质量与安全, 2010 (1): 9-12. |
| [4] | LV T, CARVALHO P N, CASAS M E, et al. Enantioselective uptake, translocation and degradation of the chiral pesticides tebuconazole and imazalil by Phragmites australis[J]. Environmental Pollution, 2017, 229: 362-370. |
| [5] | KODAMA S, YAMAMOTO A, OHURA T, et al. Enantioseparation of imazalil residue in orange by capillary electrophoresis with 2-hydroxypropyl-β-cyclodextrin as a chiral selector[J]. Journal of Agricultural and Food Chemistry, 2003, 51(21): 6128-6131. |
| [6] | PAN C X, XU X Z, ZHANG X J, et al. Comparative study of the enantioseparation of uniconazole and imazalil by HPLC on various cellulose chiral columns[J]. Analytical Letters, 2006, 39(3): 631-638. |
| [7] | 骆冲, 黄聪灵, 朱富伟, 等. 两种叶菜中5种典型手性农药对映体的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法研究[J]. 分析测试学报, 2018, 37(3): 294-299. |
| [8] | 崔璇, 钟青, 张新忠, 等. 农产品中手性农药对映体残留色谱法分析研究进展[J]. 分析测试学报, 2019, 38(2): 249-262. |
| [9] | CHASI T, YANG W, QIU J, et al. Direct enantioseparation of nitrogen-heterocyclic pesticides on cellulose-based chiral column by high-performance liquid chromatography[J]. Chirality, 2015, 27(1): 32-38. |
| [10] | LI R N, DONG F S, XU J, et al. Enantioseparation of imazalil and monitoring of its enantioselective degradation in apples and soils using ultrahigh-performance liquid chromatography-tandem mass spectrometry[J]. Journal of Agricultural and Food Chemistry, 2017, 65(16): 3259-3267. |
| [11] | 张圆圆, 刘磊, 李娜, 等. 农药残留检测中不同蔬菜的基质效应[J]. 农药学学报, 2019, 21(3): 327-337. |
| [12] | 王琦, 岳宁, 李晓慧, 等. QuEChERS技术结合超高效液相-串联质谱同时测定薄皮甜瓜中7种葫芦素[J]. 食品科学, 2022, 43(4): 144-149. |
| [13] | ORFANIDI A, GIKA H, THEODORIDIS G, et al. Development of a UHPLC-MS/MS method for the determination of 84 pharmaceuticals and drugs of abuse in human liver[J]. Journal of Chromatography B, Analytical Technologies in the Biomedical and Life Sciences, 2020, 1151: 122192. |
| [14] | LIU T, FANG K, LIU Y, et al. Enantioselective residues and toxicity effects of the chiral triazole fungicide hexaconazole in earthworms (Eisenia fetida)[J]. Environmental Pollution, 2021, 270: 116269. |
| [15] | 徐子婷, 郝莉花, 马静, 等. QuEChERS-SPE-超高效液相色谱-串联质谱法测定调味面制品中的12种真菌毒素[J]. 食品工业科技, 2022, 43(6): 311-319. |
| [16] | LI Y, NIE J Y, CHANG W X, et al. Enantioselective behavior analysis of chiral fungicide tetraconazole in apples with UPLC-MS/MS[J]. Food Control, 2020, 116: 107305. |
| [17] | LI Y, NIE J, ZHANG J, et al. Chiral fungicide penconazole: absolute configuration, bioactivity, toxicity, and stereoselective degradation in apples[J]. Science of the Total Environment, 2022, 808: 152061. |
| [18] | 刘维屏, 叶璟, 张安平, 等. 植物与手性化合物的对映体选择性相互作用[J]. 应用生态学报, 2008, 19(2): 441-448. |
| [19] | 姚周麟, 章虎, 吴韶辉, 等. 抑霉唑手性异构体及其代谢物在柑橘贮藏中的选择性行为[J]. 农药学学报, 2022, 24(1): 142-151. |
| [20] | CHANG W, NIE J, YAN Z, et al. Systemic stereoselectivity study of etoxazole: stereoselective bioactivity, acute toxicity, and environmental behavior in fruits and soils[J]. Journal of Agricultural and Food Chemistry, 2019, 67(24): 6708-6715. |
| [21] | 刘娜, 潘兴鲁, 杨庆喜, 等. 粉唑醇在草莓生长和加工过程中对映体选择性降解行为规律[J]. 食品科学, 2018, 39(24): 297-302. |
| Viewed | ||||||
|
Full text |
|
|||||
|
Abstract |
|
|||||
