液相色譜在線凈化電噴霧串聯質譜應用（二）

致。

3.3 線性方程、相關系數、檢測限（LOD）和定量限（LOQ）的測定

在選定的條件下，獲得了八種大環內酯藥物標準曲線的線性方程、相關系數和檢測限數據如表2所示。

3.4 回收率的測定

3.4.1 不同添加濃度的回收率通過以上各表可以發現本文用于提取水產品中的大環內酯類抗生素的方法，除替米卡星外，回收率穩定在60～130％之間，精密度小于12％，完全滿足日常分析檢驗的需要。

4.結 論

本文通過在線凈化建立了水產品中大環內酯類和林可胺類抗生素的高效液相色譜－電噴霧串聯質譜(LC-ESIMS/MS)檢測方法。藥物殘留的檢測限( S/N = 3)為0.1-0.2μg/kg，定量限為 1.0 μg/kg。大部分藥物在2.0～200 ng/mL時峰強度與質量濃度的線性關系良好(R2> 0.99)。在1.0、2.0、5.0、10.0 μg/kg四個添加水平下,大環內酯類的平均回收率范圍為64 %～110 %，相對標準偏差小于11.7 %。結果表明，該法簡單、靈敏，通用性好，適用于水產品中大環內酯類殘留的分析確證。

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Determination of Macrolide and lincoamide Antibiotic

Residues in aquatic products by LC-ESI-MS/MS with online

cleanup

Jinzhong Xu 1*, Xiaogong Chu 2, Xiaozhong Hu3, Tao Ding 1,

Bin Wu 1, Chongyu Shen 1, Yuan Jiang 1,

(1.Jiangsu Import & Export Inspection and Quarantine Bureau,

Nanjing 210001; 2. Chinese Academy of Inspection and

Quarantine, Beijing 100123; 3. Hubei Import & Export Inspection

and Quarantine Bureau, Wuhan 430022)

Abstract: An analytical method for the determination of

the macrolide and lincoamide antibiotic residues in aquatic

products was developed with on-line cleanup. The procedure

extracted the erythromycin(ERM), roxithromycin (ROM),

tilmicosin (TIL), tylosin(TYL), kitasamycin(KIT), josamycin(JOS),

oleandomycin(OLM), spiramycin I (SPM-I), lincomycin(LIN)

and clindamycin(CLD) from different aquatic product samples.

The macrolide and lincoamide residues were subsequently

separated and cleaned up by the reversed-HPLC and analyzed

by electrospray mass spectrometric detection. The average

recoveries for the macarolides ranged from 64 to 114% in

replicate sets of honey samples fortified with drug concentration

of 1.0, 2.0, and 10.0μg/Kg, and the relative standard deviation

(RSD) were under the 11.7% for intra-day. The method detection

limit and quantitaion limit were 0.1-0.2 μg/kg and 1.0 μg/kg,

respectively.

Keywords: Macrolides antibiotic, aquatic products, residue，

on-line clean up, LC-ESI-MS/MS