• Title/Summary/Keyword: Extraction time

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Development and Validation of the Determination of Sorafenib in Human Plasma using Tandem Mass Spectrometry Coupled with Liquid Chromatography (고속액체크로마토그래피 텐덤질량분석기법을 이용한 사람 혈장 내 소라페닙 농도분석법의 개발 및 검정)

  • Park, Daejin;Lee, Sunggon;Kim, Woomi
    • Journal of Life Science
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    • v.22 no.11
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    • pp.1456-1462
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    • 2012
  • Sorafenib is a multikinase inhibitor and an oral anticancer drug approved for the treatment of patients with advanced renal cell carcinoma and those with unresectable hepatocellular carcinoma. The purpose of this study was to develop an efficient method of the determination of sorafenib in human plasma using tandem mass spectrometry coupled with liquid chromatography (LC/MS/MS) and validate the method by the guidelines of the Korean Food and Drug Administration (KFDA). Plasma samples ($100{\mu}l$) were added with chlorantraniliprole as an internal standard and then mixed with the 0.1% formic acid-containing extraction solution composed of isopropyl alcohol and ethyl acetate (1:4, v/v). After centrifugation, the supernatant was concentrated at $45^{\circ}C$ under negative pressure and centrifugal force. The residue was reconstituted with a mobile phase and injected into the HPLC instrument using a reverse phase Waters XTerra$^{TM}$ C18 column (particle size $3.5{\mu}m$). Liquid chromatography was carried out within the run time of 5 min using a mobile phase composed of buffer (0.1% formic acid and 10 mM ammonium formate), methanol, and acetonitrile (1:6:3, v/v/v). The analytes were monitored by tandem mass spectrometry in the multiple reaction monitoring method programmed to detect sorafenib at 'm/z 465.2 ${\rightarrow}$ 252.5' and chlorantraniliprole at 'm/z 484.4 ${\rightarrow}$ 286.2' with positive electrospray ionization mode ($ES^+$). The result showed the proper linearity ($r^2$ > 0.99) over the range of 2,000-5,000 ng/ml with good accuracy (90.7-103.9%) and precision (less than 10%). The newly developed method using LC/MS/MS was validated by the guideline of KFDA and identified as more sensitive compared to the previous methods.

Analysis of Characterization in Commercial Extra Virgin Olive Oils (유통 압착올리브유의 이화학적인 특성)

  • Nam, Ha-Young;Lee, Ki-Teak
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.36 no.7
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    • pp.866-873
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    • 2007
  • To analyze and differentiate volatile compounds of 13 extra virgin olive oils from market, solid-phase micro extraction (SPME) GC-MS and electronic nose (EN) equipped with metal oxide sensors were applied. The volatiles identified in extra virgin olive oils include hexanal, 4-hexen-1-ol, (Z)-3-hexen-1-ol, acetic acid, and 2,4-dimethyl-heptane, etc. Response from EN was analysed by the principal component analysis. Proportion of the first Principal component was 99.70%, suggesting that each aroma pattern of the 13 extra virgin olive oils could be discriminated by EN. Fatty acid compositions were oleic (61.1${\sim}$77.9 mole%), palmitic (11.7${\sim}$16.5 mole%), linoleic (4.7${\sim}$9.7 mole%), stearic (2.5${\sim}$2.9 mole%), Palmitoleic (0.8${\sim}$2.4 mole%), and linolenic acid (0.7${\sim}$1.2 mole%). In color study, extra virgin olive oil showed $L^{\ast}$ value of 81.7${\sim}$92.9, $a^{\ast}$ value of -28.3${\sim}$13.5 and $b^{\ast}$ value of 52.2${\sim}$139.0. Total phenol and ${\alpha}-tocopherol$ contents were 6.2${\sim}$24.9 mg/100 g and 5.5${\sim}$12.8 mg/100 g, respectively. In Rancimat test, the induction period of 13 extra virgin olive oils showed 31.76${\sim}$54.04 hr while their POV ranged from 13.5 to 22.9 meq/kg oil.

A Study on Comparison of Characteristics of Fermentability and Fermented Broth for Houttuynia Cordata Thunb Extracts (어성초 추출물의 발효적성 및 발효액의 특성 비교)

  • Kim, Mi-Lim
    • Food Science and Preservation
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    • v.16 no.1
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    • pp.122-127
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    • 2009
  • This study was to separate wild yeast from the Houttuynia Cordata Thunb(HC) extracts fermented in traditional way and investigate the characteristics of fermentation from the HC extracts. As a result, the longer the cultivation time, the more the contents of alcohol in $15^{\circ}Brix$ sugar solutions increased. When it reached to 90 hours since it cultivated, it ranked HCE 12%, HCD 11.2%, and HCA 10.5% in order. As for HCF, HCG, HCB, and HCC), this study has shown that the contents of alcohol were from 7.5% through 8.5%. As a result of selecting germ strains like HCE and HCD with the highest alcohol-genicity in the sugar solutions as separated yeast from HC and of comparing and reviewing the existing Saccharomyces germ strains and fermentation power in the medium of HC(Juice extraction of HC : Distilled water(1:1), this study has found out that 'pH' decreased from $4.09{\sim}4.12$ before fermentation through $3.57{\sim}3.78$ after fermentation. And, the sugar concentration decreased from $15.00{\sim}15.19^{\circ}Brix$ through $7.75{\sim}9.57^{\circ}Brix$ before fermentation. Also, the acid value increased from $0.138{\sim}0.210%$ before fermentation through $0.282{\sim}0.45%$ after fermentation. In addition, as the contents of alcohol became $3.6{\sim}4.6%$ after fermentation, isolates HCD and HCE from HC had higher value rather than ones of DJ97, YJK, R12, and RCY separated from persimmons, apples, and grapes. The result value of color was minimum $4.75{\pm}1.44$ and maximum $6.85{\pm}1.63$, and HCE marked the highest record among the items of sensory evaluation. The overall acceptability was in normal level like minimum $3.95{\pm}1.17$ and maximum $5.00{\pm}1.41$. It is considered as it could lower sensory evaluation because the acceptability of flavor was not satisfied. After all, the significance(p<0.05) among the germ strains was not recognized in aspects of color, flagrance, flavor, and overall acceptability.

LP-M, a Novel Butanol-Extracts Isolated from Liriope platyphylla, could Induce the Neuronal Cell Survival and Neuritic Outgrowth in Hippocampus of Mice through Akt/ERK Activation on NGF Signal Pathway (맥문동(Liriope platyphylla)의 새로운 부탄올 추출물인 LP-M이 Akt/ERK NGF receptor signaling pathway를 통해 뇌조직에서 신경세포의 생존과 성장에 미치는 영향에 관한 연구)

  • Nam, So-He;Choi, Sun-Il;Goo, Jun-Seo;Kim, Ji-Eun;Lee, Yoen-Kyung;Hwang, In-Sik;Lee, Hye-Ryun;Lee, Young-Ju;Lee, Hong-Gu;Choi, Young-Whan;Hwang, Dae-Youn
    • Journal of Life Science
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    • v.21 no.9
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    • pp.1234-1243
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    • 2011
  • Liriope platyphylla has been used in oriental medicine as an effective medical plant to improve symptoms of cough, sputum production, neurodegenerative disorders, obesity and diabetes for long time. In order to investigate the effects of novel extracts on nerve growth factors (NGF)-stimulated neuritic outgrowth, the alteration of NGF expression and NGF receptor signaling pathway were detected in neuroblastoma cells and C57BL/6 mice. Of a total of 13 novel extracts, 4 extracts (LP-E, LP-M, LP-M50, LP2E17PJ) showed high viability on MTT assay. Also, all of these extracts induced NGF secretion and NGF mRNA expression in neuroblastoma cells. However, the NGF-induced neuritic outgrowth from PC12 cells was only stimulated by LP-E, LP-M and LP-M50. Furthermore, we selected LP-M as a best candidate, based on method and amounts of extraction, in order to verify its effect in mice. C57BL/6 mice were treated with 50 mg/kg of LP-M for 2 weeks and the effects on NGF regulation were analyzed with various methods. The expression of NGF mRNA was significantly increased in LP-M treated mice compared to vehicle treated mice. Also, the signaling pathway of p75NTR was inhibited in the cortex by LP-M treatment, with no change in the hippocampus of brain. However, the signaling pathway of TrkA was dramatically activated in only hippocampus via LP-M treatment. Therefore, these results suggest that the novel four extracts of L. platyphylla may contribute to the regulation of NGF expression and secretion in neuronal cells. LP-M was especially considered to be an excellent candidate for a neurodegenerative disease-therapeutic drug.

Characterization on the Behavior of Heavy Metals and Arsenic in the Weathered Tailings of Songcheon Mine (송천광산의 풍화광미 내 중금속 및 비소 거동 특성)

  • Lee, Woo-Chun;Kim, Young-Ho;Cho, Hyen-Goo;Kim, Soon-Oh
    • Journal of the Mineralogical Society of Korea
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    • v.23 no.2
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    • pp.125-139
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    • 2010
  • Behavior of heavy metals and arsenic in the tailings of Songcheon Au-Ag mine was characterized via both mineralogical and geochemical methods. Mineral composition of the tailings was investigated by X-ray diffractometry, energy-dispersive spectroscopy, and electron probe micro-analyzer (EPMA) and total concentrations of heavy metals and arsenic and their chemical forms were analyzed by total digestion of aqua regia and sequential extraction method, respectively. The results of mineralogical study indicate that the tailings included mineral particles of resinous shape mainly consisting of galena, sphalerite, pyrite, quartz, and scorodite, and specifically socordite was identified in the form of matrix. EPMA quantitative analyses were performed to evaluate the weatherability of each mineral, and the results suggest that it decreased in the sequence of arsenopyrite > galena > sphalerite > pyrite. The weathering pattern of galena was observed to show distinctive zonal structure consisting of secondary minerals such as anglesite and beudantite. In addition, almost all of arsenopyrite has been altered to scorodite existing asmatrix and galena, sphalerite, and pyrite which have lower weatherability than arsenopyrite were identified within the matrix of scorodite. During the process of alteration of arsenopyrite into scorodite, it is likely that a portion of arsenic was lixiviated and caused a great deal of detrimental effects to surrounding environment. The results of EPMA quantitative analyses verify that the stability of scorodite was relatively high and this stable scorodite has restrained the weathering of other primary minerals within tailings as a result of its coating of mineral surfaces. For this reason, Songcheon tailings show the characteristics of the first weathering stage, although they have been exposed to the surface environment for a long time. Based on the overall results of mineralogical and geochemical studies undertaken in this research, if the tailings are kept to be exposed to the surface environment and the weathering process is continuous, not only hazardous heavy metals, such as lead and arsenic seem to be significantly leached out because their larger portions are being partitioned in weakly-bound (highly-mobile) fractions, but the potential of arsenic leaching is likely to be high as the stability of scorodite is gradually decreased. Consequently, it is speculated that the environmental hazard of Songcheon mine is significantly high.

Geomicrobiological Behavior of Heavy Metals in Paddy Soil Near Abandoned Au-Ag Mine Supplied with Carbon Sources (탄소원을 공급한 폐금은광산 주변 논토양 내 중금속의 지구미생물학적 거동 연구)

  • Ko, M.S.;Lee, J.U.;Park, H.S.;Shin, J.S.;Bang, K.M.;Chon, H.T.;Lee, J.S.;Kim, J.Y.
    • Economic and Environmental Geology
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    • v.42 no.5
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    • pp.413-426
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    • 2009
  • The study was conducted to investigate the effects of indigenous bacteria on geochemical behavior of toxic heavy metals in contaminated paddy soil near an abandoned mine. The effects of sulfate amendment to stimulate microbial sulfate reduction on heavy metal behaviors were also investigated. Batch-type experiments were performed with lactate or glucose as a carbon source to activate indigenous bacteria in the soil under anaerobic condition for 100 days. Sulfate (250 mg/L) was artificially injected at 60 days after the onset of the experiments. In the case of glucose supply, solution pH increased from 4.8 to 7.6 while pH was maintained at 7~8 in the lactate solution. The initial low pH in the case of glucose supply likely resulted in the enhanced extraction of Fe and most heavy metals at the initial experimental period. Lactate supply exerted no significant difference on the amounts of dissolved Zn, Pb, Ni and Cu between microbial and abiotic control slurries; however, lower Zn, Pb and Ni and higher Cu concentrations were observed in the microbial slurries than in the controls when glucose supplied. Sulfate amendment led to dramatic decrease in dissolved Cr and maintenance of dissolved As, both of which had gradually increased over time till the sulfate injection. Black precipitates formed in solution after sulfate amendment, and violarite($Fe^{+2}{Ni^{+3}}_2S_4$) was found with XRD analysis in the microbial precipitates. Conceivably the mineral might be formed after Fe(III) reduction and microbial sulfate reduction with coprecipitation of heavy metal. The results suggested that heavy metals which can be readily extracted from contaminated paddy soils may be stabilized in soil formation by microbial sulfate reduction.

Quality Characteristics of Citrus Fruits According to the Harvest Date and Variety (제주산 감귤류의 품종 및 수확시기별 품질특성)

  • Song, Eun-Young;Choi, Young-Hun;Kang, Kyung-Hee;Koh, Jeong-Sam
    • Applied Biological Chemistry
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    • v.40 no.5
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    • pp.416-421
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    • 1997
  • Physicochemical properties of six cultivars of Cheju citrus fruits were investigated according to the harvest date. The fruit index of Citrus. unshiu Marc. var. miynawa, C. $natsudaidai{\;}H_{AYATA}$ and C. sudachi ranged from 1.14 to 1.38 with oval form. The fruit index of C. grandis OSEECK, C. aurantiun LINN and C. platymamma. Hort. SWINGLE ranged from 0.89 to 1.03 with a round form. The fruit weight showed the heaviest in C. grandis, followed by C. natsudaidai, C. aurantiun, C. unshiu, C. platymamma and C. sudachi. The rate of flesh showed the highest in C. unshiu, followed by C. platymamma, C. nat녀daidai, C. sudachi, C. grandis and C. aurantiun. The ratio of juice showed the highest in C. unshiu, followed by C. sudachi, C. platymamma., C. natsudaidai,, C. grandis, C. aurantiun. C. unshiu and C. platymamma, which showed a possibility to be used as raw materials for juices. The soluble solid and the Brix/acid ratio of all the varieties increased as the fruits ripen. Especially those of C. unshiu and C. platymamma were high(10.39, 7.67) in full ripe compared to other varieties. Acid content of C. natsudaidai, C. aurantiun, C. grandis and C. sudachi was sustained higher than $3{\sim}5%$ from the middle of September to the middle of January, and there was the possibility of manufacturing aromatic products like citrus vinegar. The C. sudachi contained the highest content of vitamin C,77.48 mg/100 g. The correlation between vitamin C extraction and season was insignificant. Rind and color value of all varieties were investigated, and the value of the L, a and b increased as the fruits were ripen. The value of a of rind of C. $natsudaidai{\;}H_{AYATA}$ and C. grandis until the end of November was negative. This means that their color was not presented by November since the chlorophyll was in the rind, unlike the colors of the rind of C. unshiu, C. sudachi and C. platymamma which were completed by that time.

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Improvement of an Simultaneous Determination for Clenbuterol and Ractopamine in Livestock Products using LC-MS/MS (LC-MS/MS를 이용한 축산물 중 clenbuterol과 ractopamine의 동시 분석법 개선)

  • Cho, Yoon-Jae;Chae, Young-Sik;Kim, Jae-Young;Kim, Hyung-Soo;Kang, Ilhyun;Do, Jung-Ah;Oh, Jae-Ho;Kwon, Kisung;Chang, Moon-Ik
    • Korean Journal of Food Science and Technology
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    • v.45 no.1
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    • pp.25-33
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    • 2013
  • Clenbuterol and ractopamine, which are ${\beta}$-agonists, have been misused as a growth promoting agent in meat producing animals. Clenbuterol was banned for veterinary drug in Korea because of its problems regarding safety. Due to their adverse effects, such as cardiovascular and central nervous diseases on human health proper control and monitoring should be conducted. The existing analytical method of clenbuterol and ractopamine in the Food code was improved through our present study. The bovine muscle samples were subjected to enzymatic hydrolysis, extracted with ethyl acetate and defatted by hexane-methanol partitioning. A molecular imprinted polymer (MIP) solid phase extraction cartridge was used for clean-up and LC-MS/MS was operated in positive multiple reaction monitoring (MRM). Clenbuterol-$d_9$ and ractopamine-$d_3$ were used as an internal standard. The renewed method was validated according to the CODEX guideline. The limits of quantitation for clenbuterol and ractopamine were 0.2 and 0.5 ${\mu}g/kg$, respectively. The mean recoveries ranged in 104.2-113.5% for clenbuterol and in 107.6-118.1% for ractopamine. The improved method was able to save both time and expenses.

Effect of Maturity Scores and Number of Extractions on the Chemical Properties of Water Extract from Hanwoo Shank Bones (한우 성숙도와 추출횟수가 사골용출액의 화학적 특성에 미치는 영향)

  • Kim, Jin-Hyoung;Cho, Soo-Hyun;Seong, Pil-Nam;Hah, Kyung-Hee;Jeong, Jin-Hyung;Lim, Dong-Gyun;Park, Beom-Young;Lee, Jong-Moon;Kim, Dong-Hun;Ahn, Chong-Nam
    • Food Science of Animal Resources
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    • v.27 no.4
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    • pp.463-468
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    • 2007
  • This study was conducted to investigate the effect of maturity scores [2 (bull), 2 (steer), 3-9 (cow)] and the number of extractions (up to 4 times) on the chemical properties of water extract from Hanwoo shank bones (arm, fore shank, round and hind shank). The turbidity, meat color (CIE L value), collagen, protein, caloric and chondroitin sulfate contents of samples were observed. The turbidity and lightness were higher for water extract of Hanwoo shank bones with a maturity score of 2 (bull and steer) than maturity scores of 3-9 (cow) (p<0.05). The turbidity and lightness of water extract from shank bones of all Hanwoo maturity scores significantly increased with the 1st and 2nd extractions, but significantly decreased with 3rd and 4th extractions (p<0.05). The collagen and protein contents were highest for water extract from Hanwoo shank bones of maturity score 2 (bull and steer) (p<0.05). The caloric and chondroitin sulfate contents were higher for water extract from Hanwoo shank bones of maturity score 2 (bull and steer) than maturity scores of 3-9 (cow) (p<0.05). As the number of extractions increased, the chondroitin sulfate content significantly decreased (p<0.05). Based on these results, differences correlating with maturity scores were found only with collagen and protein contents. Therefore, further studies should be considered to address whether different maturity scores affect the price of shank bones in the meat industry.

Identification of Fatty Acids in the Pulp Oils of Jujube and Their Compsitional Changes in the Ripening Period (대추의 과육지질(果肉脂質)에 존재(存在)하는 지방산(脂肪酸)의 동정(同定)과 숙성(熟成)에 따른 그 조성(組成)의 변화(變化))

  • Woo, Hyo-Kyeng;Kim, Seong-Jin;Park, Sung-Hea;Joh, Yong-Goe
    • Journal of the Korean Applied Science and Technology
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    • v.18 no.1
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    • pp.67-77
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    • 2001
  • In search for several fatty acid with unusual structure in vegetable oils, we have found that unknown peaks were shown on GLC in the analysis of fatty acids of the lipids from the pulp of ripened jujube (Zizypus jujuba var. inermis) fruits. These fatty acids were identified as a series of cis-monoenoic acids with ${\omega}-5$ double bond system such as $C_{14:1{\omega}5}$, $C_{16:1{\omega}5}$ and $C_{18:1{\omega}5}$, including ${\omega}-7$ fatty acid as $C_{16:1{\omega}7}$ and $C_{18:1{\omega}7}$, by GLC, solid-phase extraction silver ion-column chromatographic, GLC-mass spectrometric and IR techniques. First of all, total fatty acid methyl esters were resolved into saturated and branched fatty acid, monoenoic acid, dienoic acid, and trienoic acid fraction, respectively, with 100% dichloromethane (DCM), DCM/acetone (9:1, v/v) 100% acetone, and acetone/ acetonitrile (97:3, v/v) solvent system. Unknown fatty acids were included in the monoenoic fraction and were confirmed to have cis-configuration by IR. Picolinyl esters of monoenoic fatty acids gave distinct molecular ion peak and dominant diagnostic peaks, for example, m/z 317, 220 and 260 fragment for $cis-C_{14:1{\omega}5}$, m/z 345, m/z 248 and 288 fragment for $cis-C_{16:1{\omega}5}$ and m/z 373, m/z 276 and 316 fragment for $cis-C_{18:1{\omega}5}$. In this way the occurrence of $cis-C_{16:1{\omega}7}$ and $cis-C_{18:1{\omega}7}$ could be deduced from the appearance of prominent fragments as m/z 345, 220 and 260, and m/z 373, 248 and 280. Level of total ${\omega}-5$ fatty acids amounted to about 30% in the fatty acid composition with the predominance of $C_{16:1{\omega}5}$ $ (18.7{\sim}25.0%)$, in the semi-ripened and/or ripened samples collected in September 14 ($C_{16:1{\omega}5}$ ; 18.7%, $C_{14:1{\omega}5}$ ; 3.6% and $C_{18:1{\omega}5}$ ; 3.0%), September 22 ($C_{16:1{\omega}5}$ ; 25.0%, $C_{14:1{\omega}5}$ ; 1.4% and $C_{18:1{\omega}5}$ ; 2.6%), and October $7 (C_{16:1{\omega}5}$ ; 24.7%, $C_{14:1{\omega}5}$ ; 7.7% and $C_{18:1{\omega}5}$ ; 2.5%). However, the lipids extracted from unripened jujube in July and August contain these unusual fatty acids as low as negligible. It could be observed that the level of ${\omega}-5$ fatty acids in the pulps increased sharply with an elapse of ripening time of jujube fruits. Other monoenoic fatty acids with ${\omega}-7$ series, $C_{16:1{\omega}7}$ (palmitoleic acid) and $C_{18:1{\omega}7}$ (cis-vaccenic acid) could be detected. And in the lipids of the kernel and leaf of jujube, none of ${\omega}-5$ fatty acids could be detected.