• Journal of Food Hygiene and Safety
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• v.36 no.3
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• pp.228-238
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• 2021

The aim of this research was to develop a rapid and easy multi-residue method for determining dimethipin, omethoate, dimethipin, chlorfenvinphos and azinphos-methyl in agricultural products (hulled rice, potato, soybean, mandarin and green pepper). Samples were prepared using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and analyzed using gas chromatography-tandem mass spectrometry (GC-MS/MS). Residual pesticides were extracted with 1% acetic acid in acetonitrile followed by addition of anhydrous magnesium sulfate (MgSO₄) and anhydrous sodium acetate. The extracts were cleaned up using MgSO₄, primary secondary amine (PSA) and octadecyl (C₁₈). The linearity of the calibration curves, which waas excellent by matrix-matched standards, ranged from 0.005 mg/kg to 0.3 mg/kg and yielded the coefficients of determination (R²) ≥ 0.9934 for all analytes. Average recoveries spiked at three levels (0.01, 0.1, 0.5 mg/kg) and were in the range of 74.2-119.3%, while standard deviation values were less than 14.6%, which is below the Codex guideline (CODEX CAC/GL 40).

• Journal of Food Hygiene and Safety
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• v.37 no.3
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• pp.136-142
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• 2022

The research aims to develop a rapid and easy analytical method for methoprene using liquid chromatography-tandem mass spectrometry (LC-MS/MS). A simple, highly sensitive, and specific analytical method for the determination of methoprene in livestock products (beef, pork, chicken, milk, eggs, and fat) was developed. Methoprene was effectively extracted with 1% acetic acid in acetonitrile and acetone (1:1), followed by the addition of anhydrous magnesium sulfate (MgSO₄) and anhydrous sodium acetate. Subsequently, the lipids in the livestock sample were extracted by freezing them at -20℃. The extracts were cleaned using MgSO₄, primary secondary amine (PSA), and octadecyl (C₁₈), which were then centrifuged to separate the supernatant. Nitrogen gas was used to evaporate the supernatant, which was then dissolved in methanol. The matrix-matched calibration curves were constructed using 8 levels (1, 2.5, 5, 10, 25, 50, 100, 150 ng/mL) and the coefficient of determination (R²) was above 0.9964. Average recoveries spiked at three levels (0.01, 0.1, and 0.5 mg/kg), and ranged from 79.5-105.1%, with relative standard deviations (RSDs) smaller than 14.2%, as required by the Codex guideline (CODEX CAC/GL 40). This study could be useful for residue safety management in livestock products.

• Journal of Food Hygiene and Safety
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• v.38 no.4
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• pp.211-216
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• 2023

A total of 100 commercially available olive oil products were analyzed for 179 pesticide residues using gas chromatography-tandem mass spectrometry (GC/MS/MS). The olive oil samples were mixed with organic solvents, centrifuged and frozen to remove fat, and pesticide residues were analyzed using the "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) method. The determination coefficient (R²) of the analysis method used in this study was ≥0.998. The detection limit of the method ranged 0.004-0.006 mg/kg and its quantitative limit ranged 0.012-0.017 mg/kg. The recovery rate (n=5) measured at the level ranging 0.01-0.02, 0.1, and 0.5 mg/kg ranged 66.8-119.5%. The relative standard deviation (RSD) was determined to be ≤5.7%, confirming that this method was suitable for the "Guidelines for Standard Procedures for Preparing Food Test Methods". The results showed that a total of 151 pesticides (including difenoconazole, deltamethrin, oxyfluorfen, kresoxim-methyl, phosmet, pyrimethanil, tebuconazole, and trifloxystrobin) were detected in 64 of the 100 olive oil products. The detection range of these pesticide residues was 0.01-0.30 mg/kg. The percentage acceptable daily intake (%ADI) of the pesticides calculated using ADI and estimated daily intake (EDI) was 0.0001-0.1346, indicating that the detected pesticides were present at safe levels. This study provides basic data for securing the safety of olive oil products by monitoring pesticide residues in commercially available oilve oil products. Collectively, the analysis method used in this study can be used as a method to analyze residual pesticides in edible oils.

• Analytical Science and Technology
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• v.22 no.6
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• pp.488-497
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• 2009

In this study, analytical methodology for several organic fatty acids (OFA: propionic acid (PA), butyric acid (BA), isovaleric acid (IA), and valeric acid (VA)) designated as new offensive odorants in Korea (as of year 2010) was investigated along with some odorous VOCs (styrene, toluene, xylene, methyl ethyl ketone, methyl isobutyl ketone, butyl acetate, and isobutyl alcohol). For this purpose, working standards (WS) containing all of these 13 compounds were loaded into adsorption tube filled with Tenax TA, and analyzed by gas chromatography (GC) system thermal desorber interfaced with. The analytical sensitivities of organic fatty acids expressed in terms of detection limit (both in absolute mass (ng) and concentration (ppb)) were lower by 1.5-2 times than other compounds (PA: 0.24 ng (0.16 ppb), BA: 0.19 ng (0.11 ppb), IA: 0.15 ng (0.07 ppb), and VA: 0.28 ng (0.13 ppb)). The precision of BA, IA, and VA, if assessed in terms of relative standard error (RSE), maintained above 5%, while the precison of other compounds were below 5%. The reproducibility of analysis improved with the aid of internal standard calibration (PA: $1.1{\pm}0.4%$, BA: $10{\pm}0.46$, IA; $12{\pm}0.3%$, VA: $4{\pm}0.1%$), respectively. The results of this study showed that organic fatty acid can be analyzed using adsorption tube and thermal desorber in a more reliable way to replace alkali absorption method introduced in the odor prevention law of the Korea Ministry of Environment (KMOE).

• KOREAN JOURNAL OF CROP SCIENCE
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• v.4 no.1
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• pp.1-23
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• 1968

This study aimed at contributing to the improvement of cropping systems after finding out the effects of excrements and components of crop root influence on other crops as well as themselves. The following forage crops suitable for our country were selected for the present study. Aqueous extracts of fresh roots, aqueous extracts of rotting roots and aqueous solutions of excrements of red clover, orchard grass and brome grass were studied for the effects influencing the germination and growth of seedlings of red clover, ladino clover, lespedeza, soybean, orchard grass, Italian ryegrass, brome grass, barley, wheat, sorghum, corn and Hog-millet. In view of the possibility that the organic acid might be closely related to the excrements and components of crop root connected with soil sickness, the acid components of three species of roots were analysed by paper chromatography and gas chromatography method. The following results were obtained: 1. Effects of Aqueous Extracts of Fresh Roots : Aqueous extracts of red clover: The extracts inhibited the growth of seedlings of the ladino clover and lespedeza and also inhibited the development of most crops except that of sorghum among the Graminaceae. Aqueous extracts of orchard grass: The extracts promoted the seedlings growth of red clover and soybean, while it inhibited the germination and growth of orchard grass. There were no noticeable effects influencing other crops while it inhibited the growth of barley and Hog-millet. Aqueous extracts of brome grass: There was no effect on Italian ryegrass but there was an inhibiting effect on the other crops. 2. Effects of Aqueous Extracts of Rotting Roots : Aqueous extracts of red clover: The extracts promoted the seedling growth of red clover. But it reflected the inhibiting effects on other crops except sorghum. Aqueous extracts of orchard grass: The extracts promoted the growth of red clover, ladino clover, soybean and sorghun, while it inhibited the germination and rooting of barley and Hog-millet. Aqueous extracts of brome grass: The extracts gave the promotive effects to the growth of red clover, soybean and sorghum, but caused inhibiting effects on orchard grass, brome grass, barley and Hog-millet. 3. Effects of Aqueous Solutions of Excrements : The aqueous solution of excrements of red clover reflected the inhibition effects to the growth of Graminaceae, while the aqueous solutions of excrements of orchard grass and Italian ryegrass caused the promotive effects on the growth of red clover. 4. Results of Organic Acid Analysis : The oxalic acid, citric acid, tartaric acid, malonic acid, malic acid and succinic acid were included in the roots of red clover as unvolatile organic acid, and in the orchard grass and brome grass there were included the oxalic acid, citric acid, tartaric acid and malic acid. And formic acid was confirmed in the red clover, orchard grass and brome grass as volatile organic acid. In consideration of the results mentioned in above the effects of excrements and components of roots found in this studies may be summarized as follows. 1) The red clover generally gave a disadvantageous effect on the Graminaceae. Such trend was considered chiefly caused by the presence of many organic acids, namely oxalic, citric, tartaric, malonic, malic, succinic and formic acid. 2) The orchard grass generally gave an advantageous effect on the Leguminosae. This may be due to a few kinds of organic acid contained in the root, namely oxalic, citric, tartaric, malic and formic acid. Furthermore a certain of promotive materials for growth was noted. 3) As long as the root of brome grass are not rotten, it gave a disadvantageous effect on the Leguminosae and Graminaceae. This may be due to the fact that several unidentified volatile organic acid were also included besides the confirmed organic acid, namely oxalic, citric, tartaric, malic and formic acid. 5. Effects of Components in Roots to the Soil Sickness : 1) It was considered that the cause of alleged red clover's soil sickness did not result from the toxic components of the roots. 2) It was recognized that the toxic components of roots might be the cause of soil sickness in case the orchard grass and brome grass were put into the long-term single cropping. 6. Effects of Rooted Components to the Companion Crops in the Cropping System : a) In case of aqueous extracts of fresh roots and aqueous excrements (Inter cropping and mixed cropping) : 1) Advantageous combinations : Orchard grass->Red clover, Soybean, Italian ryegrass->Red clover, 2) Disadvantageous combinations : Red clover->Ladino clover, Lespedeza, Orchard grass, Italian ryegrass, Fescue Ky-31, Brome grass, Barley, Wheat, Corn and Hog.millet, Orchard grass->Lespedeza, Orchard grass, Barley and Hog-millet, Brome grass->Red clover, Ladino clover, Lespedeza, Soybean, Orchard grass, Brome grass, Barley, Wheat, Sorghum, Corn and Hog-millet, 3) Harmless combinations : Red clover->Red clover, Soybean and Sorghum, Orchard grass->Ladino clover, Italian ryegrass, Brome grass, Wheat, Sorghum and Corn, Brome grass->Italian ryegrass, b) In case of aquecus extracts of rotting roots(After cropping) : 1) Advantageous combinations : Red clover->Red clover and Sorghum, Orchard grass->Red clover, Ladino clover, Soybean, Sorghum, and Corn, Brome grass->Red clover, Soybean and Sorghum, 2) Disadvantageous combinations : Red clover->Lespedeza, Orchard grass, Italian ryegrass, Brome grass, Barley, Wheat, and Hog-millet Orchard grass->Barley and Hog-millet, Brome grass->Orchard grass, Brome grass, Barley and Hog-millet, 3) Harmless combinations : Red clover->Ladino clover, Soybean and Corn, Orchard grass->Lespedeza, Orchard grass, Italian ryegrass, Brome grass and Wheat Brome gass->Ladino clover, Lespedeza, Italian ryegrass and Wheat.

• The Korean Journal of Pesticide Science
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• v.18 no.3
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• pp.130-140
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• 2014

Recently, some of the previous studies reported that tolclofos-methyl is still exist in ginseng cultivated soil, even though it is has been banned for ginseng. Therefore, the current study was aimed to examine the levels of absorption and translocation of tolclofos-methyl from ginseng cultivated soil to ginseng root and leaf stem for the period of 1 year. For this study, ginseng plants were transplanted in pots and treated with $5.0mg\;kg^{-1}$ of tolclofos-methyl (50% WP). At the end of each interval periods (every three months) the samples (soil, roots and leaf stems) were collected and analyzed the absorption and translocation levels of tolclofos-methyl using gas chromatography and mass spectrometry (GC-MS). The limit of quantitation of tolclofos-methyl was found to be $0.02mg\;kg^{-1}$ and 70.0~120.0% recovery was obtained with coefficient of variation of less than 10% regardless of sample types. In this study, a considerable amount of translocation of tolclofos-methyl residues were found in soil (4.28 to $0.06mg\;kg^{-1}$), root (7.09 to $1.54mg\;kg^{-1}$) and leaf stem (0.79 to $0.69mg\;kg^{-1}$). The results show that the tolclofos-methyl was absorbted and translocated from ginseng cultivated soil to ginseng root and ginseng leaf stem and found to be decreased time-coursely. Secondly, we were also analyzed soil, root and leaf stems samples from Hongcheon, Cheorwon, Punggi and Geumsan by GC-MS/MS (172 pesticides), LC-MS/MS (74 pesticides). In this study, 43 different pesticides were detected ($0.01{\sim}7.56mg\;kg^{-1}$) in soil, root and leaf stem. Further, tolclofos-methyl was detected 4 times separately in root sample alone which is less ($0.01{\sim}0.05mg\;kg^{-1}$) than their maximum residual limit (MRL) in ginseng. Consequently, the results from both studies indicate the residues of tolclofos-methyl found in ginseng cultivated soil and ginseng ensuring their safety level. Moreover, long-term evaluations are needed in order to protect the soil as well as ginseng free from tolclofos-methyl residues.

• Journal of the Korean Applied Science and Technology
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• v.13 no.1
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• pp.21-29
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• 1996

Levels of total, neutral and polar lipids from the seeds of eight species of the Cucurbitaceae f Cucurbita moschata, Lufa cylindrica, Citrullus vulgari, Cucumis melo var. makuwa, Cucumis satvus, Lag leucantha. Trichosanthes kirilowii and Momordica charantia, were determinded, and their fatty compositions were also analyzed by gas-liquid chromatography. The results were summarized as foll. Lipid contents of the seeds range from 21.9 to 50.7%, which contained 98% up of neutral lipi the fatty acid compositon of ottal lipids from the seeds of Cucurbita moschata, Lufa cylindrica, Ci vulgari, Cucumis melo var. makuwa, Cucumis sativus and Lagenaria leucantha, linoleic acid is the mos dominant component(56.8${\sim}$84.0%) followed by oleic acid(5.7${\sim}$22.2%) and palmitic acid(6.1${\sim}$1) with a trace amount of ${\alpha}-linolenic$ acid(below 0.6%). On the contrary, the seed oils of Tricho kirilowii and Momordica charantia are characterized by presence of considerable amounts of con trienoic acid such as punicic acid($_{9c.11t.13c-}C_{18:3}$) and ${\alpha}-eleostearic$ acid($_{9c.11t.13c-}C_{18:3}$). For example total lipids of T. kirilowii seeds were mainly composed of linoleic acid(40.5%) and punicic acid(3) in the fatty acid composition, while those of M. charantia seeds predominantly comprised ${\alpha}-eleos$ acid as a main component(66.9%), accompanied by oleic acid(11.7%) and linoleic acid(10.4%). oil ${\beta}-eleostearic$ acid($_{9t.11t.13c-}C_{18:3}$) was checked as a trace. Fatty acid profiles of neutral lipids close resemblance to those of total lipids in all the seed oils, but are different from those of polar In particular, conjugate trienoic acids including punicic acid and ${\alpha}-eleostearic$ acid which are oc as the most abundant component in both neutral lipids of T. kirilowii and M. charantia seed oils, ar ent in a extremely small amount in both polar lipids. The fatty acid distribution in the polar lipid the samples except for T. kirilowii and M. charantia seed oils, showed a tendency of consid increased level of saturated fatty acids(25.0${\sim}$29.4%) compared with that in the neutral lipids(9.9%). The results obtained in this experiment suggest us that the seed oils of the Cucurbitaceae

• The Korean Journal of Nuclear Medicine Technology
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• v.22 no.2
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• pp.67-73
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• 2018

$[^{11}C]PIB$ synthesis has been performed by a loop-methylation and HPLC purification in our lab. However, this method is time-consuming and requires complicated systems. Thus, we developed an on-cartridge method which simplified the synthetic procedure and reduced time greatly by removing HPLC purification step. We compared 6 different cartridges and evaluated the $[^{11}C]PIB$ production yields and specific activities. $[^{11}C]MeOTf$ was synthesized by using TRACERlab FXC Pro and was transferred into the cartridge by blowing with helium gas for 3 min. To remove byproducts and impurities, cartridges were washed out by 20 mL of 30% EtOH in 0.5 M $NaH_2PO_4$ solution (pH 5.1) and 10 mL of distilled water. And then, $[^{11}C]PIB$ was eluted by 5 mL of 30% EtOH in 0.5 M $NaH_2PO_4$ into the collecting vial containing 10 mL saline. Among the 6 cartridges, only tC18 environmental cartridge could remove impurities and byproducts from $[^{11}C]PIB$ completely and showed higher specific activity than traditional HPLC purification method. This method took only 8 ~ 9 min from methylation to formulation. For the tC18 environmental cartridge and conventional HPLC loop methods, the radiochemical yields were $12.3{\pm}2.2%$ and $13.9{\pm}4.4%$, respectively, and the molar activities were $420.6{\pm}20.4GBq/{\mu}mol$ (n=3) and $78.7{\pm}39.7GBq/{\mu}mol$ (n=41), respectively. We successfully developed a facile on-cartridge methylation method for $[^{11}C]PIB$ synthesis which enabled the procedure more simple and rapid, and showed higher molar radio-activity than HPLC purification method.

• Journal of Korean Society of Forest Science
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• v.32 no.1
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• pp.36-63
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• 1976

The purpose of this study is to elucidate the genetic variation of the natural forest of Pinus densiflora. Three natural populations of the species, which are considered to be superior quality phenotypically, were selected. The locations and conditions of the populations are shown in table 1 and 2. The morphological traits of tree and needle and some other characteristics were presented already in our first report of this series in which population and family differences according to observed characteristics were statistically analyzed. Twenty trees were sampled from each populations, i.e., 60 trees in total. During the autumn of 1974, matured cones were collected from each tree and open-pollinated seeds were extracted in laboratory. Immediately after cone collection, in closed condition, the morphological characteristics were measured. Seed and seed-wing dimensions were also studied. In the spring of 1975, the seeds were sown in the experimental tree nursery located in Suweon. And in the April of 1976, the 1-0 seedlings were transplanted according to the predetermined experimental design, randomized block design with three replications. Because of cone setting condition. the number of family from which progenies were raised by populations were not equal. The numbers of family were 20 in population 1. 18 in population 2 and 15 in population 3. Then, each randomized block contained seedlings of 53 families from 3 populations. The present paper is mainly concerned with the variation of some characteristics of cone, seed, needle, growth performance of seedlings, and chlorophyll and monoterpene compositions of needles. The results obtained are summerized as follows. 1. The meteorological data obtained by averaging the records of 30 year period, observed from the nearest station to each location of populations, are shown in Fig. 3, 4, and 5. The distributional pattern of monthly precipitation are quite similar among locations. However, the precipitation density on population 2, Seosan area, during growing season is lower as compared to the other two populations. Population 1. Cheong-song area, and population 3, Pyong-chang area, are located in inland, but population 2 in the western seacoast. The differences on the average monthly air temperatures and the average monthly lowest temperatures among populations can hardly be found. 2. Available information on the each mother trees (families) studied, such as age, stem height, diameter at breast height, clear-bole-length, crown conditions and others are shown in table 6,7, and 8. 3. The measurements of fresh cone weight, length and the widest diameter of cone are given in Tab]e 9. All these traits arc concerned with the highly significant population differences and family differences within population. And the population difference was also found in the cone-index, that is, length-diameter ratio. 4. Seed-wing length and seed-wing width showed the population differences, and the family differences were also found in both characteristics. Not discussed in this paper, however, seed-wing colours and their shapes indicate the specificity which is inherent to individual trees as shown in photo 3 on page 50. The colour and shape are fully the expression of genetic make up of mother tree. The little variations on these traits are resulted from this reason. The significant differences among populations and among families were found in those characteristics, such as 1000-seed weight, seed length, seed width, and seed thickness as shown in table 11. As to all these dimensions, the values arc always larger in population 1 which is younger in age than that of the other two. The population differences evaluated by cone, seed and seed-wing sizes could partly be attributed to the growth vigorousity. 5. The values of correlation between the characteristics of cone and seed are presented in table 12. As shown, the positive correlations between cone diameter and seed-wing width were calculated in all populations studied. The correlation between seed-wing length and seed length was significantly positive in population 1 and 3 but not in population 2, that is, the r-value is so small as 0.002. in the latter. The correlation between cone length and seed-wing length was highly significant in population 1, but not in population 2. 6. Differences among progenies in growth performances, such as 1-0 and 1-1 seedling height and root collar diameter were highly singificant among populations as well as families within population(Table 13.) 7. The heritability values in narrow sense of population characteristics were estimated on the basis of variance components. The values based on seedling height at each age stage of 1-1 and 1-0 ranged from 0.146 to 0.288 and the values of root collar diameter from 0.060 to 0.130. (Table 14). These heritability values varied according to characteristics and seedling ages. Here what must be stated is that, for calculation of heritability values, the variance values of population was divided by the variance value of environment (error) and family and population. The present authors want to add the heritability values based on family level in the coming report. It might be considered that if the tree age is increased in furture, the heritability value is supposed to be altered or lowered. Examining the heritability values studied previously by many authors, in pine group at age of 7 to 15, the values of height growth ranged from 0.2 to 0.4 in general. The values we obtained are further below than these. 8. The correlation between seedling growth and seed characteristics were examined and the values resulted are shown in table 16. Contrary to our hypothetical premise of positive correlation between 1-0 seedling height and seed weight, non-significance on it was found. However, 1-0 seedling height correlated positively with seed length. And significant correlations between 1-0 and 1-1 seedling height are calculated. 9. The numbers of stomata row calculated separately by abaxial and adaxial side showed highly significant differences among populations, but not in serration density. On serration density, the differences among families within population were highly significant. (Table 17) A fact must be noted is that the correlation between stomata row on abaxial side and adaxial side was highly significant in all populations. Non-significances of correlation coefficient between progenies and parents regarding to stomata row on abaxial side were shown in all populations studied.(Table 18). 10. The contents of chhlorophyll b of the needle were a little more than that of chlorophyll a irrespective of the populations examined. The differences of chlorophyll a, b and a plus b contents were highly significant but not among families within populations as shown in table 20. The contents of chlorophyll a and b are presented by individual trees of each populations in table 21. 11. The occurrence of monoterpene components was examined by gas liquid chromatography (Shimazu, GC-1C type) to evaluate the population difference. There are some papers reporting the chemical geography of pines basing upon monoterpene composition. The number of populations studied here is not enough to state this problem. The kinds of monoterpene observed in needle were ${\alpha}$-pinene, camphene, ${\beta}$-pinene, myrcene, limonene, ${\beta}$-phellandrene and terpinolene plus two unknowns. In analysis of monoterpene composition, the number of sample trees varied with population, I.e., 18 families for population 1, 15 for population 2 and 11 for population3. (Table 22, 23 and 24). The histograms(Fig. 6) of 7 components of monoterpene by population show noticeably higher percentages of ${\alpha}$-pinene irrespective of population and ${\beta}$-phellandrene in the next order. The minor Pinus densiflora monoterpene composition of camphene, myrcene, limonene and terpinolene made up less than 10 percent of the portion in general. The average coefficients of variation of ${\alpha}$-pinene and ${\beta}$-phellandrene were 11 percent. On the contrary to this, the average coefficients of variation of camphene, limonene and terpinolene varied from 20 to 30 percent. And the significant differences between populaiton were observed only in myrcene and ${\beta}$-phellandrene. (Table 25).