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CASE
Determination of sulfonamides in milk with pressurized capillary electrochromatography based on sub-micron stationary phase
Keywords: Sub-micron C18 bonded silica particle stationary phase; Pressurized capillary
electrochromatography; Electroosmotic flow; Sulfonamides
electrochromatography; Electroosmotic flow; Sulfonamides
Details
Abstract: An improved Stber method was used to prepare the sub-micron particles of 780 nm and 830 nm for uniformly packed columns． Compared with the regular chromatography medium of 1. 8μm and 3 μm，the percentage of EOF in whole velocity was larger with smaller particle size． The packed capillary column with 780 nm C18 bonded silica particles was applied in the determination of five sulfonamides in milk． The five sulfonamides were completely separated in 5 minutes． The results indicated that the linear rang was 0. 1 ～ 10. 0 mg/L (Ｒ 2 ≥0. 9990)，the limit of detection was 0. 02 ～ 0. 04 mg/L， and the average recovery was 86. 5% ～ 98. 8% ( except for sulfonamide)．
Chromatographic packing is developing towards smaller particle size The decrease of particle size also causes the problem of high back pressure. When chromatographic packing When the column is sub 2 μ m, the back pressure is high even if the effective column length is only 5 cm Therefore, the performance of the sub micron chromatographic packing was in the high performance liquid phase The development of HPLC is limited. But the pressure capillary Tube electrochromatography (pCEC) combines HPL C and capillary electrophoresis(CE) has the advantages of dual drive of pressure flow and electroosmotic flow It can effectively solve the problem of high back pressure, which is the development of submicron chromatographic packing The exhibition provi des a broader platform.
Sulfonamides are widely used in animal husbandry. Human consumption contains Sulfonamides are harmful to health［4，5］ 。 our country Document No. 235 issued in 2002 stipulates sulfonamides in food The residue should not exceed 100 μ g / L [6]. Sulfonamides residues The common detection methods are liquid chromatography tandem mass spectrometry (LC-MS) [7,8], liquid chromatography fluorescence detection (lc-fld) [9,10] and liquid chromatography Ultraviolet Detection (LC-UV) [11,12]. LC-MS has high sensitivity, but the equipment is expensive and the cost is high [13]; lc-fld requires derivatization of samples, and the pretreatment process is complex and cumbersome [14]; LC-UV is the most widely used, but there are also problems such as longer gradient elution detection time [15]. At present, the packing particle sizes of commercial C1 chroma tographic columns for the detection of sulfonamides are mostly 3 μ m and 5 μ M.
In this study, submicron Beige was synthesized by improved St BER method A highly uniform packed capillary column was prepared The contribution rate of electroosmotic flow (EOF) in submicron chromatographic column was investigated This method can be applied to a capillary column packed with conventional 1.8 μ m and 3 μ m chromatographic media Comparison was made to illustrate the sub micron chromatographic medium in pCEC mode The advantages and characteristics of. A submicron capillary column was used in this study Based on pCEC platform, five sulfonamides residues in milk were established The method of solid phase extraction and pCEC detection was used.
conclusion
A highly uniform packed submicron capillary column was prepared,8 μ m and 3 μ m stationary phases It was found that the smaller the particle size of the stationary phase was, the higher the electroosmotic flow rate was The greater the contribution rate. Combining the advantages of submicron packing and pCEC platform,A solid phase extraction (SPE) method was developed for the determination of 5 sulfonamides in milk- The detection method of pCEC is the detection of sulfonamides residues A fast and effective method is provided. The method will be further applied to the determination of other sulfonamides residues in milk,At the same time, the corresponding pretreatment method is also provided for other actual samples Amine drug residues were detected, such as milk powder, water samples, animal derived food Products, etc.conclusion A highly uniform packed submicron capillary column was prepared,8 μ m and 3 μ m stationary phases It was found that the smaller the particle size of the stationary phase was, the higher the electroosmotic flow rate wasThe greater the contribution rate. Combining the advantages of submicron packing and pCEC platform,A solid phase extraction (SPE) method was developed for the determination of 5 sulfonamides in milk-The detection method of pCEC is the detection of sulfonamides residues A fast and effective method is provided. The method will be further applied to the determination of other sulfonamides residues in milk,At the same time, the corresponding pretreatment method is also provided for other actual samples Amine drug residues were detected, such as milk powder, water samples, animal derived food Products, etc.
Chromatographic packing is developing towards smaller particle size The decrease of particle size also causes the problem of high back pressure. When chromatographic packing When the column is sub 2 μ m, the back pressure is high even if the effective column length is only 5 cm Therefore, the performance of the sub micron chromatographic packing was in the high performance liquid phase The development of HPLC is limited. But the pressure capillary Tube electrochromatography (pCEC) combines HPL C and capillary electrophoresis(CE) has the advantages of dual drive of pressure flow and electroosmotic flow It can effectively solve the problem of high back pressure, which is the development of submicron chromatographic packing The exhibition provi des a broader platform.
Sulfonamides are widely used in animal husbandry. Human consumption contains Sulfonamides are harmful to health［4，5］ 。 our country Document No. 235 issued in 2002 stipulates sulfonamides in food The residue should not exceed 100 μ g / L [6]. Sulfonamides residues The common detection methods are liquid chromatography tandem mass spectrometry (LC-MS) [7,8], liquid chromatography fluorescence detection (lc-fld) [9,10] and liquid chromatography Ultraviolet Detection (LC-UV) [11,12]. LC-MS has high sensitivity, but the equipment is expensive and the cost is high [13]; lc-fld requires derivatization of samples, and the pretreatment process is complex and cumbersome [14]; LC-UV is the most widely used, but there are also problems such as longer gradient elution detection time [15]. At present, the packing particle sizes of commercial C1 chroma tographic columns for the detection of sulfonamides are mostly 3 μ m and 5 μ M.
In this study, submicron Beige was synthesized by improved St BER method A highly uniform packed capillary column was prepared The contribution rate of electroosmotic flow (EOF) in submicron chromatographic column was investigated This method can be applied to a capillary column packed with conventional 1.8 μ m and 3 μ m chromatographic media Comparison was made to illustrate the sub micron chromatographic medium in pCEC mode The advantages and characteristics of. A submicron capillary column was used in this study Based on pCEC platform, five sulfonamides residues in milk were established The method of solid phase extraction and pCEC detection was used.
conclusion
A highly uniform packed submicron capillary column was prepared,8 μ m and 3 μ m stationary phases It was found that the smaller the particle size of the stationary phase was, the higher the electroosmotic flow rate was The greater the contribution rate. Combining the advantages of submicron packing and pCEC platform,A solid phase extraction (SPE) method was developed for the determination of 5 sulfonamides in milk- The detection method of pCEC is the detection of sulfonamides residues A fast and effective method is provided. The method will be further applied to the determination of other sulfonamides residues in milk,At the same time, the corresponding pretreatment method is also provided for other actual samples Amine drug residues were detected, such as milk powder, water samples, animal derived food Products, etc.conclusion A highly uniform packed submicron capillary column was prepared,8 μ m and 3 μ m stationary phases It was found that the smaller the particle size of the stationary phase was, the higher the electroosmotic flow rate wasThe greater the contribution rate. Combining the advantages of submicron packing and pCEC platform,A solid phase extraction (SPE) method was developed for the determination of 5 sulfonamides in milk-The detection method of pCEC is the detection of sulfonamides residues A fast and effective method is provided. The method will be further applied to the determination of other sulfonamides residues in milk,At the same time, the corresponding pretreatment method is also provided for other actual samples Amine drug residues were detected, such as milk powder, water samples, animal derived food Products, etc.
