| 第 51 卷第 5 期 |  | Vol. 51 No. 5 | | 2021 年 10 月 | Oct 2021 |
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所屬欄目：分析與測試
硝基聯(lián)苯、氨基聯(lián)苯及啶酰菌胺的高效液相色譜分析方法 |
| 高 翀1，陸亞軍1，龐懷林2
（1. 上海泰禾化工有限公司，上海201612；2. 南通泰禾化工股份有限公司，江蘇 南通 226407） |
| 摘 要：建立了一種高效液相色譜定量方法，測定以4-氯-2'-硝基聯(lián)苯制備4-氯-2'-氨基聯(lián)苯合成啶酰菌胺路線(xiàn)各步反應中的有效成分含量。采用InertSustain ODS-C18 不銹鋼柱（250 mm×4.6 mm i.d.×5 μm）和二極管陣列檢測器，以乙腈和0.02%磷酸水為流動(dòng)相，流速為1.0 mL／min，在220 nm波長(cháng)下對中間體4-氯-2'-硝基聯(lián)苯進(jìn)行分離和定量分析；在254 nm波長(cháng)下對中間體4-氯-2'-氨基聯(lián)苯進(jìn)行分離和定量分析；在254 nm波長(cháng)下對啶酰菌胺進(jìn)行分離和定量。分析結果表明，4-氯-2'-硝基聯(lián)苯保留時(shí)間約24.3 min，線(xiàn)性相關(guān)系數為1.000 0，標準偏差為0.04，變異系數為0.34%，平均回收率為100.04%；4-氯-2'-氨基聯(lián)苯保留時(shí)間約18.0 min，線(xiàn)性相關(guān)系數為1.000 0，標準偏差為0.05，變異系數為0.33%，平均回收率為99.94%；啶酰菌胺保留時(shí)間約11.9 min，線(xiàn)性相關(guān)系數為1.000 0，標準偏差為0.21，變異系數為0.32%，平均回收率為100.09%。方法操作簡(jiǎn)便，精密度與準確度較高，滿(mǎn)足定量分析要求。 |
| 關(guān)鍵詞：啶酰菌胺；4-氯-2'-硝基聯(lián)苯；4-氯-2'-氨基聯(lián)苯；高效液相色譜 |
| 中圖分類(lèi)號：O657.7+2 文獻標識碼：A 文章編號：1009-9212（2021）05-0096-06 |
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| HPLC Analysis of Nitrobiphenyl, Aminobphenyl and Boscalid |
| GAO Chong1, LU Ya-Jun1, PANG Huai-lin2
(1. CAC Shanghai Chemicals Co., Ltd., Shanghai 201612, China; 2. CAC Nantong Chemicals Co., Ltd., Nantong 226407, China) |
| Abstract：A HPLC method was established for determination of active ingredients in each reaction step of the synthetic route in which 4-chloro-2'-amino biphenyl was prepared from 4-chloro-2'-nitrobiphenyl and used to synthesize Boscalid. The sample was separated and analyzed using Eclipse ODS-C18 stainless steel column (250 mm×4.6 mm i.d.×5 μm) equipped with UV detector at 220 nm for 4-chloro-2'-nitrobiphenyl, while a wavelength of 254 nm was set for the determination of 4-chloro-2'-amino biphenyl and Boscalid. A mixture of acetonitrile and 0.02% phosphoric acid solution was used as the mobile phase with a flow rate of 1.0 mL/min. Results showed the fpllowings: the retention time (RT) of 4-chloro-2'-nitrobiphenyl was 24.3 min; the linear correlation coefficient (R2) was 1.000 0; the standard deviation(SD) was 0.04; the variation coefficient (CV) was 0.34%; and average recovery was 100.04 %; the RT of 4-chloro-2'-amino biphenyl was 18.0 min with a R2 of 1.0000, SD of 0.05; CV was of 0.33%; and average recovery was 99.94%. The RT of Boscalid was of 11.9 min, while the R2 was 1.000 0; SD was of 0.21; CV was of 0.32%; and average recovery of 100.09%. This method is of high accuracy, short time, and convenience. |
| Key words：Boscalid; 4-chloro-2'-nitrobiphenyl; 4-chloro-2'-amino biphenyl; HPLC |
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作者簡(jiǎn)介：高 翀（1985—），男，上海人，研究方向：農藥及精細化工分析（E-mail：chong_gao@cacch.com）。
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收稿日期：2021-08-03
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