干旱区生态环境知识资源中心(Arid): 全自动固相萃取-高效液相色谱法测定熟肉制品中3种红曲色素的含量

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	全自动固相萃取-高效液相色谱法测定熟肉制品中3种红曲色素的含量
其他题名	HPLC Determination of 3 Monascus Pigments in Cooked Meat Products with Automatic-SPE
	傅红雪; 陈万勤; 刘柱; 周霞; 罗金文; 梁晶晶
来源期刊	理化检验. B, 化学分册
ISSN	1001-4020
出版年	2019
卷号	55 期号:10 页码:1132-1136
中文摘要	取熟肉样品5.000 g,用乙醇-水(85+15)溶液25.0 mL超声提取15 min,在4 ℃下快速离心10 min。移取上清液10.0 mL,加入乙醇30 mL,在(602) ℃下旋转蒸发至近干,用甲醇-水(20+80)溶液5.0 mL分2次溶解残渣,将所得溶液通过全自动固相萃取仪的Oasis HLB SPE柱(500 mg/6 mL),并按程序进行自动净化富集处理,收集洗脱液在40 ℃下吹氮至近干。用乙醇-水(85+15)溶液2.0 mL溶解残渣,所得溶液经0.22 m滤膜过滤后作为待测液进行高效液相色谱分析。用Waters SunFire C_(18)色谱柱(250 mm*4.6 mm,5 m)作为固定相,进样量为20 L,流动相由甲醇和20 mmol·L~(-1)乙酸铵溶液按不同比例混合组成,按程序进行3种红曲色素(红曲红胺的检测波长为264 nm,红曲素和红曲红素的检测波长均为390 nm)的分离和测定,采用二极管阵列检测器测定。用3种红曲色素的混合标准溶液系列按方法操作制得3种组分的标准曲线,其相关系数均在0.999 5以上。以3倍信噪比计算得3种组分的检出限(3S/N)依次为0.20,0.060,9.9 mg·kg~(-1)。以空白样品作为基体,按照标准加入法进行回收试验,测得回收率在92.9%~100 %之间,测定值的相对标准偏差(n =6)在1.3 %~3.7 %之间。
英文摘要	The meat sample (5.000 g) was extracted ultrasonically with 25.0 mL of ethanol-H_2O (85+15) solution for 15 min, and the mixture was centrifuged at 4 ℃ for 10 min at high speed. The supernatant (10.0 mL) was taken and added with 30 mL of ethanol. The solution was evaporated to near-dryness at (60+2) ℃. The residue was taken up with 2 portions of methanol-H_2O (20+80) solution,using 2.5 mL in each dissolution. The analytes of 3 monascus pigments in the methanol solution were then purified and enriched by passing the solution through Oasis HLB SPE column (500 mg/6 mL) of the automatic-SPE installation and operated according to the program automatically. The eluate was collected and evaporated to near-dryness by N2-blowing at 40 ℃. The residue was dissolved with 2.0 mL of C2 H_5OH-H_2O (85+15) solution and after filtering through 0.22 m filtering membrane, the filtrate was used as testing solution for HPLC analysis. Waters SunFire C_(18) chromatographic column (250 mm*4.6 mm, 5 m) was used as stationary phase and mixtures with various ratios of methanol and 20 mmol·L~(-1) NH_4 OAc solution were used as mobile phases in the programed gradient elution for separation of the 3 monascus pigments and their determinations with diode array detector, at wavelengths of 264 nm for monascorubramine and at 390 nm for both monascin and monascorubrin. Linearity ranges between definite mass concentrations of the 3 monascus pigments were obtained having their correlation coeffcients greater than 0.999 5. Detection limits (3S/N) found for the 3 monascus pigments were 0.20, 0.060,9.9 mg·kg~(-1) respectively. Test for recovery was made by standard addition method using a blank sample as matrix,the results obtained were in the range of 92.9% -100%. Values of RSDs (n = 6) were found range from 1.3% -3.7%.
中文关键词	全自动固相萃取 ; 高效液相色谱法 ; 红曲色素 ; 熟肉制品
英文关键词	automatic-SPE HPLC monascus pigment cooked meat product
类型	Article
语种	中文
收录类别	CSCD
WOS类目	Chemistry
CSCD记录号	CSCD:6607894
资源类型	期刊论文
条目标识符	http://119.78.100.177/qdio/handle/2XILL650/353244
作者单位	傅红雪, 浙江省食品药品检验研究院, 杭州, 浙江 310052, 中国. 陈万勤, 浙江省食品药品检验研究院, 杭州, 浙江 310052, 中国. 刘柱, 浙江省食品药品检验研究院, 杭州, 浙江 310052, 中国. 周霞, 浙江省食品药品检验研究院, 杭州, 浙江 310052, 中国. 罗金文, 浙江省食品药品检验研究院, 杭州, 浙江 310052, 中国. 梁晶晶, 浙江省食品药品检验研究院, 杭州, 浙江 310052, 中国.
推荐引用方式 GB/T 7714	傅红雪,陈万勤,刘柱,等. 全自动固相萃取-高效液相色谱法测定熟肉制品中3种红曲色素的含量[J],2019,55(10):1132-1136.
APA	傅红雪,陈万勤,刘柱,周霞,罗金文,&梁晶晶.(2019).全自动固相萃取-高效液相色谱法测定熟肉制品中3种红曲色素的含量.理化检验. B, 化学分册,55(10),1132-1136.
MLA	傅红雪,et al."全自动固相萃取-高效液相色谱法测定熟肉制品中3种红曲色素的含量".理化检验. B, 化学分册 55.10(2019):1132-1136.