Microsoft Word 钱勇-二校

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1 6 7 Vol. 6 No Journal of Food Safety and Quality Jul., 2015 Ⅰ Ⅱ 钱勇 1*, 许纪锋 1, 诸晨 1, 沈君子 1, 金金花 2, 梅利中 2, 谢天培 3 (1., ; 2., ; 3., ) 摘要 : 目的 (high performance liquid chromatography, HPLC), 方法 90%, Ultimate XB-C 18 (4.6 mm 250 mm, 5 μm), : =32:68 (V:V)(0.1% ), 1.0 ml/min, 35, 440 nm 结果 15~300 μg/ml (r 2 =0.9996), 96.6%, RSD 1.69%; 12~240 μg/ml (r 2 =0.9998), 96.1%, RSD 1.58%, 结论, 关键词 : ; Ⅰ; Ⅱ; ; Determination of crocusⅠand crocusⅡin saffron QIAN Yong 1*, XU Ji-feng 1, ZHU Chen 1, SHEN Jun-Zi 1, JIN Jin-Hua 2, MEI Li-Zhong 2, SXIE Tian-Pei 3 (1. Shanghai Standard Biotech Co., Ltd., Shanghai , China; 2. Shanghai Huapu Medicine Decoction Pieces Co., Ltd., Shanghai , China; 3. Shanghai 100 Standard Testing Co., Ltd., Shanghai , China) ABSTRACT: Objective To develop a method for determination of crocus Ⅰ and crocus Ⅱ in saffron by high performance liquid chromatography (HPLC), and compare the content of crocusⅠand crocus Ⅱ in different saffron. Methods The saffron was extracted by ultrasonic in 90% ethanol solution. Separations of extraction solution were carried out on an Ultimate XB-C 18 (4.6 mm 250 mm, 5 μm). The mobile phase(volume rate)was ACN:H 2 O = 32:68 (V:V) (0.1% methanoic acid), the flow was 1.0 ml/min, column temperature was 35, and the detection wavelength was 440 nm. Results Crocus Ⅰ had a good linearity with the peak areas in 15~300 μg/ml (r 2 =0.9996). The average recovery was 96.6% and the RSD was 1.69%. Crocus Ⅱ had a good linearity with the peak areas in 12~240 μg/ml(r 2 =0.9998). The average recovery was 96.1% and the RSD was 1.58%. The difference of content of crocus Ⅰ and crocus Ⅱ was obvious in different cultivated fields. Conclusion This method is simple, sensitive, specific, and reproducible, which can be used as the method for measuring the content of crocus Ⅰ and crocus Ⅱ in saffron. KEY WORDS: saffron; crocus Ⅰ; crocus Ⅱ; high performance liquid chromatography; determination of content 基金项目 : ( ) Fund: Supported by the Science and Technology Plan of STCSM ( ) * 通讯作者 :,, qianyong2232@163.com *Corresponding author: QIAN Yong, Engineer, Shanghai Standard Biotech Co., Ltd., Building 2, Room 103, No.720, Cailun Road, Shanghai , China. qianyong2232@163.com

2 7, : Ⅰ Ⅱ 引言 (Crocus sativus L.),, B1, ; [1-3], α- [4-7], 1,,,,, [8-10], (high performance liquid chromatography, HPLC) [11-16],, HPLC, [11,12,16] 1 Ⅰ(1) Ⅱ(2) Fig. 1 Structure of crocusⅠ(1) and crocus Ⅱ (2)

3 2824 6, Ⅱ, Ⅰ Ⅱ,, 2 材料与方法 2.1 材料与试剂 ( 98.5%, ), (, ),, (, ), (, ) 2.2 仪器与设备 Agilent1260, Chemstation ( ); ( ); ELGA ( ); HS-800D ( ); Fresco-21 ( ) 2.3 方法过程色谱条件 : Ultimate XB- C18(4.6 mm 250 mm, 5 μm), : : =32:68 (V:V)( 0.1% ) 1.0 ml/min, 440 nm, 对照品溶液的制备 15.0 mg 12.0 mg 25 ml,,, 0.60 mg/ml, 0.48 mg/ml 2 Fig. 2 Liquid chromatogram of saffron (1: Ⅰ, 2: Ⅱ; A, B ) (1: crocusⅠ, 2: crocusⅡ; A: reference standards of crocusⅠand crocusⅡ; B: extract sample of saffron)

4 7, : Ⅰ Ⅱ 供试药材溶液的制备 0.1 g,, 100 ml, 90% 60 ml, min, 2,,,, 2 ml 10 ml,,, 0.45 μm, 3 结果与分析 3.1 线性范围的考察, μg/ml 5, 10 μl,, μg/ml 5, 10 μl, (Y), (X), : Y=36655X (r 2 =0.9996), 15~300 μg/ml ; : Y=12606X , (r 2 =0.9998) 12~240 μg/ml 3.2 精密度试验, 6, 10 μl, RSD 0.65%, RSD 0.95%, 3.3 稳定性试验, h, 7, 10 μl, RSD 0.55%, RSD 0.75%, 24 h 3.4 重现性试验 5,,, 10 μl,, 79.5 mg/g 28.6 mg/g, RSD 1.75% 1.42% 3.5 加样回收率试验 6,, ml 2,,, 10μL, 96.6% 96.1%, RSD 1.69% 1.58% 3.6 不同产地的西红花苷 Ⅰ 和西红花苷 Ⅱ 含量测定,,, 10 μl, 2,, 1 表 1 Table 1 不同产地西红花中西红花苷 Ⅰ 和西红花苷 Ⅱ 的含量 (n=3) Content of crocusⅠand crocusⅡ in different saffron (n=3) Ⅰ(%) Ⅱ(%) Ⅰ Ⅱ (%) RSD(%)(Ⅰ Ⅱ ) XHH XHH XHH XHH XHH XHH

5 Ⅰ(%) Ⅱ(%) Ⅰ Ⅱ (%) RSD(%)(Ⅰ Ⅱ ) 续表 1 XHH XHH XHH XHH XHH XHH XHH XHH XHH XHH XHH XHH XHH XHH XHH 结论与讨论 4, 21,,, [17],,, 10.0%,,,, ( 2~4 ),, [11,12,16],,,, 参考文献 [1]. ( )[M]. :, Chinese Pharmacopoeia Commission. Pharmacopoeia of the People's Republic of China (First Volume) [M]. Beijing: Chinese Medical Science and Technology Press, [2] Amin A, Hamza AA, Bajbouj K, et al. Saffron: a potential candidate for a novel anticancer drug against hepatocellular carcinoma [J]. Hepatology, 2011, 54(3): [3] Tavakkol, Afshari J, Brook A, et al. Study of cytotoxic and apoptogenie properties of saffron extract in human cancer cell lines [J]. Food Chem Toxical, 2008, 46(11): [4] Bajbouj K, Schulze-Luehrmann J, Diermeier S, et a1. The anti-cancer effect of saffron in two p53 isogenic colorectal cancer cell lines [J]. BMC Compl Altem Med, 2012, 12: 69. [5] Aung HH, Wang CZ, Ni M, et a1. Crocin from crocus sativus

7, : Ⅰ Ⅱ 2827 possesses significant anti-proliferation effects on human colorectal cancer cells [J]. Exp Oncol, 2007, 29: 175 180. [6] Abdullaev FI. Crocus sativus against cancer [J].

6 7, : Ⅰ Ⅱ 2827 possesses significant anti-proliferation effects on human colorectal cancer cells [J]. Exp Oncol, 2007, 29: [6] Abdullaev FI. Crocus sativus against cancer [J]. Arch Med Res, 2003, 34: [7] Poma A, Fontecchio G, Carlucci G, et a1. Anti-inflammatory properties of drugs from saffron crocus [J]. Antiinflamm Antiallergy Agents Med Chem, 2012, 11(1): [8],,,. [J]., 2002, 27(8): Deng Y, Guo ZG, Zeng ZL, et al. Pharmacological research progress of saffron [J]. China J TCM, 2002, 27(8): [9] Plozano MR, Castellar, Simancas MJ, et a1. Quantitative high-performance liquid chromatographic method analyses commercial saffron (Crocus sativus L.) products [J]. J Chromatogr A, 1999, 830: [10],,,. [J]., 2011, 2l(8): 914. Sun CB, Liu YX, Liu GQ, et al. Pharmacological research progress of saffron [J]. Med J Nat Defend Forces Southwest China, 2011, 2l(8): 914. [11],,. [J]., 1997, 22(11): Zhang L, Zhou JX, Zhou SD. Content determination of different introduction about the origin of Crocus sativus L. [J]. China J TCM, 1997, 22(11): [12]. [J]., 1997, (2) Zhou SD. Spectrophotometric determination of total glycosides in tablets [J]. Strait Pharm J, 1997, 9(2): 3 4. [13],,,. Ⅰ He CM, Xie XM, He ML, et al. Establishment of the measurement method of crocus I and crocus II in Crocus sativus L. [J]. Chin J Pharm Anal, 2006, 26(9): [14] Johnson TE, Hermanson D, Wang L, et al. Lung tumorigenesis suppressing effects of a commercial kava extract and its selected compounds in A/J mice [J]. Am J Chin Med, 2011, 39: [15],,,. [J]., 2011, 25(3): Zhao XJ, Zhang JJ, Pei WZ, et al. Correlation analysis between effective component contents and corm dimension of saffron [J]. Acta Univ Trad Med Sinen Pharmacol Shanghai, 2011, 25(3): 95. [16],,,. HPLC UV [J]., 2009, 2(6): Chen Y, Sun ZY, Zhang H, et al. Comparative evaluation of HPLC and UV-visible methods to quantify crocins of gardenia and saffron [J]. Food Eng, 2009, 2(6): [17],,,. [J]., 2012, 4 (12): Xu XH, Shi LM, Zhu B, et al. Different origin of Crocus sativus L. flowering and the effective composition content research [J]. Zhenjiang Agric Sci, 2012, 4 (12): 作者简介 ( 责任编辑 : 杨翠娜 ) 钱勇, 硕士研究生, 工程师, 主要研究方向为中药和健康食品的检测及化学成分研究 Qianyong2232@163. com Ⅱ [J]., 2006, 26(9):

g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min

g ml 10% ph 色谱条件 kinetex C μm 100 A 4. 6 mm 150 mm 25 5 μl A B 10 mmol /L ml /min 25 4 2013 8 监测技术 5 1 2 1 ( 1. 江苏省疾病预防控制中心, 江苏南京 210009; 2. 南京医科大学第二附属医院, 江苏南京 210029) 5 Phenomenex kinetex C 18 2. 6 μm 4. 6 mm 150 mm 10 mmol /L ph 2. 5 + 60 40 DAD 280 nm 5 20. 0 mg /L ~ 100 mg /L 0.

Microsoft Word 钱 勇-二校

Microsoft Word 钱勇-二校