分析仪器
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ANALYTICAL INSTRUMENTATION
2015年
2期
44-47
,共4页
超高效液相色谱法%喹乙醇%残留量%猪肉
超高效液相色譜法%喹乙醇%殘留量%豬肉
초고효액상색보법%규을순%잔류량%저육
UPLC%olaqunindox%residue%pork
建立了超高效液相色谱测定猪肉中喹乙醇的方法。样品温水提取,用亚铁氯化钾和乙酸锌沉淀蛋白,超高效液相色谱-紫外检测器测定。色谱柱BEH C181·7μm ×50mm ×2·1mm ,用不同体积的甲醇和水混合作为流动相梯度洗脱,检测波长380nm ;流速0·3mL/min;柱温40℃;进样量3μL。喹乙醇的质量浓度分别一定范围内与其峰面积呈线性关系,检出限(3S/N )为0·015μg/g。以空白猪肉为基体进行加标回收试验,回收率在92·3%~97·8%之间,相对标准偏差(n=6)在1·2%~2·6%之间。结论:本方法适用于猪肉中喹乙醇的测定。
建立瞭超高效液相色譜測定豬肉中喹乙醇的方法。樣品溫水提取,用亞鐵氯化鉀和乙痠鋅沉澱蛋白,超高效液相色譜-紫外檢測器測定。色譜柱BEH C181·7μm ×50mm ×2·1mm ,用不同體積的甲醇和水混閤作為流動相梯度洗脫,檢測波長380nm ;流速0·3mL/min;柱溫40℃;進樣量3μL。喹乙醇的質量濃度分彆一定範圍內與其峰麵積呈線性關繫,檢齣限(3S/N )為0·015μg/g。以空白豬肉為基體進行加標迴收試驗,迴收率在92·3%~97·8%之間,相對標準偏差(n=6)在1·2%~2·6%之間。結論:本方法適用于豬肉中喹乙醇的測定。
건립료초고효액상색보측정저육중규을순적방법。양품온수제취,용아철록화갑화을산자침정단백,초고효액상색보-자외검측기측정。색보주BEH C181·7μm ×50mm ×2·1mm ,용불동체적적갑순화수혼합작위류동상제도세탈,검측파장380nm ;류속0·3mL/min;주온40℃;진양량3μL。규을순적질량농도분별일정범위내여기봉면적정선성관계,검출한(3S/N )위0·015μg/g。이공백저육위기체진행가표회수시험,회수솔재92·3%~97·8%지간,상대표준편차(n=6)재1·2%~2·6%지간。결론:본방법괄용우저육중규을순적측정。
The target analyst was extract form samples with water ,involved protein precipitation with zinc acetate and ferrous potassium chloride. Chromatographic column:BEH C18 1.7μm × 50 mm × 2.1mm , detection wavelength :380nm ,flow rate:0.3mL/min ,column temperature:40℃ ,injection volume:3μL , and separated with mixtures of methanol and water mixed in different rations as mobile phases. Result :Linear relationships between values of peak area and concentration of olaqunindox was obtained in the defi‐nite rages ,with detection limits of(3S/N)0.05μg/g. Using samples of blank pork as matrixes ,tests for recovery were made by standard addition method ,and values of recovery were in rage of 92%‐103% ,and values of RSD’s (n= 6)were in the rage of 1.2%‐2.6% . The method is suitable for determination of olaqunindox residue in pork.