분석조건
LC기울기 용리8.2.2.2FD-수산물-중-동물용의약품-동시-다성분-시험법-x1원문 표제 단서: 액체크로마토그래프
- 칼럼
- C18 · USP L1
C18계 컬럼
안지름 2.1 mm · 길이 15 cm · 입자경 3.5 μm
- 칼럼온도
- 40℃
- 이동상
- 0.1%(v/v) 포름산(formic acid) 함유한 수용액
- 2 mM 포름산암모늄(ammonium acetate) 및 0.1% 포름산(formic acid) 함유한 아세토니트릴
- 유량
- 0.3 mL/분
- 주입량
- 5 μL
- 기타표
구분,정량한계 계열,동물용의약품,넙치,장어,새우 린코사마이드계,린코마이신,0.001,0.001,- 클린다마이신,0.005,0.005,- 마크로라이드계,스피라마이신,-,-,- 에리스로마이신,0.001,0.001,- 올레안도마이신,0.01,0.01,0.01 조사마이신,0.001,0.001,0.001 틸미코신,0.01,0.01,0.01 키타사마이신,-,-,- 벤조이미다졸계,메벤다졸,0.01,0.01,0.01 메벤다졸 아민,0.01,0.01,0.01 5-하이드록시 메벤다졸,0.01,0.01,0.01 티아벤다졸,0.01,0.01,0.01 5-하이드록시 티아벤다졸,0.01,0.01,0.01 설파계,설파구아니딘,0.005,0.005,0.005 설파독신,0.001,0.001,0.001 설파디메톡신,0.001,0.001,0.001 설파디아진,0.001,0.001,0.001 설파메라진,0.001,0.001,0.001 설파메타진,0.001,0.001,0.001 설파메톡사졸,0.001,0.001,0.001 설파메톡시피리다진,0.001,0.001,0.001 설파모노메톡신,0.001,0.001,0.001 설파퀴녹살린,0.001,0.001,0.001 설파클로르피리다진,0.001,0.001,0.001 설파클로르피라진,0.001,0.001,0.001 설파티아졸,0.001,0.001,0.001 설파페나졸,0.001,0.001,0.001 설피속사졸,0.001,0.001,0.001 세팔로스포린계,세파드록실,0.001,0.001,- 세팔렉신,0.005,0.005,0.005 세프티오퍼,-,-,- 데스후로일세프티오퍼,-,-,- 퀴놀론계,날리딕스산,0.0001,0.0001,0.0001 노르플록사신,0.0007,0.0007,0.0007 다노플록사신,0.01,0.01,0.01 디플록사신,0.001,-,- 마보플록사신,0.0001,0.0001,0.0001 시프로플록사신,0.0001,0.0001,0.0001 엔로플록사신,0.0001,0.0001,0.0001 오플록사신,0.0002,0.0002,0.0002 옥소린산,0.0001,-,0.0001 페플록사신,0.0007,0.0007,0.0007 플루메퀸,-,-,- 테트라싸이클린계,독시싸이클린,0.005,0.005,0.005 옥시테트라싸이클린,0.001,0.001,0.001 클로르테트라싸이클린,0.001,0.001,0.001 테트라싸이클린,0.001,-,0.001 미노싸이클린,0.01,-,0.01 페니실린계,벤질페니실린,0.01,0.01,0.01 아목시실린,0.005,-,- 암피실린,0.005,0.005,0.005 클록사실린,0.01,0.01,0.01 페니콜계,플로르페니콜,-,-,- 플로르페니콜 아민,-,-,- 티암페니콜,-,-,- 클로람페니콜,-,-,- 기타,데하이드로콜산,0.005,0.005,0.005 디아베리딘,0.01,0.01,0.01 비치오놀,-,-,- 에토파베이트,0.01,0.01,0.01 m-페네티딘,0.01,0.01,0.01 오르메토프림,-,-,- 트리메토프림,0.001,0.001,0.001 트리클로르폰,0.001,0.001,- 티아물린,0.001,0.001,- 페노뷰카브,0.001,0.001,0.001 푸마길린,-,-,- 프라지콴텔,0.001,0.001,0.001
질량분석(MS) 조건 보기 (5항목)
- 이온화 방법
- 가) 이온화 방법: ESI(Positive ion mode, Negative ion mode)
- Capillary temperature
- 나) Capillary temperature: 500℃
- Capillary voltage
- 다) Capillary voltage: 3.8 kV(Positive), 2.6 kV(Negative)
- Collision gas
- 라) Collision gas: 아르곤(Ar) 또는 이와 동등한 것
- 전이표
연번 분석성분 (Compound) 머무름 시간 (분) 이온화(Ionization mode) 분자량 (MW) 관측질량 (Exact mass) 선구이온 (Precusor ion, m/z) 생성이온 (Product ion, m/z) 충돌에너지 (Collision energy, eV) 1 날리딕스산 (Nalidixic acid) 6.77 Positive 232.2 232.08 233 104 187 2151) 36 25 12 2 노르플록사신 (Norfloxacin) 3.27 Positive 319.3 319.13 320 233 2761) 302 20 15 20 3 다노플록사신 (Danofloxacin) 3.56 Positive 357.4 357.14 358 231 3141) 340 30 15 20 4 데하이드로콜산 (Dehydrocholic acid) 7.41 Negative 402.5 401.10 401 2151) 249 331 30 32 23 5 독시싸이클린 (Doxycycline) 5.01 Positive 444.4 444.15 445 267 321 4281) 34 29 16 6 디아베리딘 (Diaveridine) 2.83 Positive 260.2 260.13 261 81 1231) 245 40 25 28 7 디플록사신 (Difloxacin) 4.21 Positive 399.4 399.13 400 2991) 356 382 25 20 20 8 린코마이신 (Lincomycin) 2.76 Positive 406.5 406.21 407 1261) 172 359 30 20 18 9 마보플록사신 (Marbofloxacin) 3.11 Positive 362.4 362.13 363 721) 320 345 20 15 20 10 메벤다졸 (Mebendazole) 6.46 Positive 295.2 295.09 296 104 165 2641) 30 40 20 10-1 메벤다졸 아민 (Mebendazole amine) 4.51 Positive 237.2 237.09 238 1051) 133 160 25 30 25 10-2 5-하이드록시 메벤다졸 (5-hydroxy mebendazole) 4.50 Positive 297.3 297.11 298 79 160 2661) 35 35 20 11 미노싸이클린 (Minocycline) 3.02 Positive 457.5 457.18 458 283 3521) 441 43 28 15 12 벤질페니실린 (Benzylpenicillin, Penicillin G) 6.58 Positive 334.4 334.09 335 114 1601) 176 30 15 15 13 비치오놀 (Bithionol) 10.4 Negative 356.0 354.90 355 1611) 163 194 28 28 25 14 설파구아니딘 (Sulfaguanidine) 1.13 Positive 214.2 214.05 215 60 92 1561) 12 10 5 15 설파독신 (Sulfadoxine) 5.00 Positive 310.3 310.07 311 92 108 1561) 28 24 16 16 설파디메톡신 (Sulfadimethoxine) 5.96 Positive 310.3 310.07 311 921) 108 156 28 26 18 17 설파디아진 (Sulfadiazine) 2.63 Positive 250.2 250.05 251 92 108 1561) 26 22 14 18 설파메라진 (Sulfamerazine) 3.33 Positive 264.3 264.06 265 92 108 1561) 24 22 16 19 설파메타진 (Sulfamethazine) 3.87 Positive 278.3 278.08 279 92 124 1861) 28 22 16 20 설파메톡사졸 (Sulfamethoxazole) 5.02 Positive 253.2 253.05 254 92 108 1561) 26 20 14 21 설파메톡시피리다진 (Sulfamethoxypyridazine) 3.97 Positive 280.3 280.06 281 92 108 1561) 30 25 14 22 설파모노메톡신 (Sulfamonomethoxine) 4.45 Positive 280.3 280.06 281 92 108 1561) 28 24 16 23 설파퀴녹살린 (Sulfaquinoxaline) 5.98 Positive 300.3 300.06 301 92 108 1561) 22 22 17 24 설파클로르피라진 (Sulfachlorpyrazin, Sulfaclozine) 4.66 Positive 284.7 284.01 285 92 108 1561) 26 24 14 25 설파클로르피리다진 (Sulfachlorpyridazine) 5.85 Positive 284.7 284.01 285 92 108 1561) 24 22 14 26 설파티아졸 (Sulfathiazole) 2.91 Positive 255.3 255.01 256 921) 108 156 24 22 15 27 설파페나졸 (Sulfaphenazole) 6.08 Positive 314.4 314.08 315 92 1581) 160 34 28 22 28 설피속사졸 (Sulfisoxazole) 5.33 Positive 267.3 267.06 268 92 1131) 156 31 16 14 29 세파드록실 (Cefadroxil) 1.60 Positive 363.4 363.08 364 1141) 208 15 10 30 세팔렉신 (Cefalexin) 3.14 Positive 347.4 347.09 348 106 1581) 174 26 10 14 31 세프티오퍼 (Ceftiofur) 5.57 Positive 523.6 523.02 524 95 125 2411) 42 58 16 31-1 데스후로일세프티오퍼 (Desfuroylceftiofur) 4.55 Positive 429.5 429.02 430 1281) 259 368 25 18 15 32 스피라마이신 (Spiramycin) 4.55 Positive 843.1 842.51 422 101 142 1741) 12 10 18 33 시프로플록사신 (Ciprofloxacin) 3.40 Positive 331.3 331.13 332 204 231 2451) 53 35 19 34 아목시실린 (Amoxicillin) 1.39 Positive 365.4 365.10 366 113 133 3491) 19 31 5 35 암피실린 (Ampicillin) 3.12 Positive 349.4 349.11 350 79 1061) 114 44 17 30 36 에리스로마이신 (Erythomycin) 6.16 Positive 733.9 733.46 734 82 1581) 576 35 25 18 37 에토파베이트 (Ethopabate) 5.84 Positive 237.2 237.10 238 136 164 2061) 25 20 10 37-1 m-페네티딘 (m-phenetidine) 3.04 Positive 137.1 137.08 138 65 93 1101) 20 25 10 38 엔로플록사신 (Enrofloxacin) 3.71 Positive 359.4 359.16 360 189 2451) 286 40 23 32 39 오르메토프림 (Ormethoprim) 3.48 Positive 274.3 274.14 275 81 1231) 259 43 25 27 40 오플록사신 (Ofloxacin) 3.29 Positive 361.4 361.14 362 221 2611) 318 35 28 15 41 옥소린산 (Oxolinic acid) 5.45 Positive 261.2 261.06 262 129 1601) 173 35 28 17 42 옥시테트라싸이클린 (Oxytetracycline) 3.41 Positive 460.4 460.14 461 201 337 4261) 18 40 28 43 올레안도마이신 (Oleandomycin) 5.83 Positive 687.9 687.41 688 116 1581) 544 40 25 15 44 조사마이신 (Josamycin) 7.59 Positive 828.0 827.46 828 83 1091) 174 40 45 34 45 클로람페니콜 (Chloramphenicol) 5.61 Negative 323.1 322.01 321 1521) 194 257 18 12 10 46 클로르테트라싸이클린 (Chlortetracycline) 4.77 Positive 478.9 478.11 479 98 1541) 444 40 24 22 47 클록사실린 (Cloxacillin) 7.89 Positive 435.9 435.06 436 159 178 3211) 10 20 15 48 클린다마이신 (Clindamycin) 4.98 Positive 425.0 424.17 426 1261) 335 377 25 18 15 49 키타사마이신 (Kitasamycin) 6.93 Positive 785.9 701.40 772 83 1091) 174 45 38 30 50 테트라싸이클린 (Tetracycline) 3.72 Positive 444.4 444.15 445 1541) 225 410 24 50 16 51 트리메토프림 (Trimethoprim) 3.18 Positive 290.3 290.13 291 123 2301) 261 30 18 25 52 트리클로르폰 (Trichlorfon) 4.28 Positive 257.4 255.92 259 79 1091) 223 25 18 10 53 티아물린 (Tiamulin) 6.91 Positive 493.7 493.32 494 73 1191) 192 50 40 20 54 티아벤다졸 (Thiabendazole) 2.72 Positive 201.2 201.04 202 92 131 1751) 30 25 25 54-1 5-하이드록시 티아벤다졸 (5-hydroxy thiabendazole) 1.91 Positive 217.2 217.03 218 81 108 1471) 35 30 25 55 티암페니콜 (Thiamphenicol) 3.70 Positive 356.2 355.00 354 185 240 2901) 20 16 12 56 틸미코신 (Tilmicosin) 5.39 Positive 869.1 868.56 870 88 126 1741) 60 55 45 57 페노뷰카브 (Fenobucarb) 8.63 Positive 207.2 207.13 208 57 95 1521) 15 15 5 58 페플록사신 (Pefloxacin) 3.34 Positive 333.3 333.14 334 2331) 290 316 23 16 18 59 푸마길린 (Fumagillin) 9.27 Positive 458.5 458.23 459 1311) 177 233 25 15 12 60 프라지콴텔 (Praziquantel) 8.12 Positive 312.4 312.18 313 83 174 2031) 22 28 14 61 플로르페니콜 (Florfenicol) 5.14 Negative 358.2 357.00 356 118 1851) 336 40 21 13 61-1 플로르페니콜 아민 (Florfenicol amine) 1.11 Positive 247.2 247.06 248 91 130 2301) 42 25 10 62 플루메퀸 (Flumequine) 7.03 Positive 261.2 261.08 262 991) 126 202 54 44 30
기울기 조건표
| 시간(분) | A(%) | B(%) |
|---|---|---|
| 0.0 | 90 | 10 |
| 1.0 | 90 | 10 |
| 6.0 | 60 | 40 |
| 10.0 | 5 | 95 |
| 15.0 | 5 | 95 |
| 15.1 | 90 | 10 |
| 20.0 | 90 | 10 |
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고시 원문 보기 (축자)
가) 컬럼: C18계 컬럼(2.1 mm × 150 mm, 3.5 μm) 또는 이와 동등한 것 나) 이동상 (1) 이동상 A: 0.1%(v/v) 포름산(formic acid) 함유한 수용액 (2) 이동상 B: 2 mM 포름산암모늄(ammonium acetate) 및 0.1% 포름산(formic acid) 함유한 아세토니트릴 [표 1] 다) 이동상 유량: 0.3 mL/분 라) 컬럼 온도: 40℃ 마) 주입량: 5 μL 2) 질량분석기 분석조건 가) 이온화 방법: ESI(Positive ion mode, Negative ion mode) 나) Capillary temperature: 500℃ 다) Capillary voltage: 3.8 kV(Positive), 2.6 kV(Negative) 라) Collision gas: 아르곤(Ar) 또는 이와 동등한 것 마) 분석대상물질 조건 [표 2] 1) 정량이온 3) 검량선 작성 4) 정량한계 (단위: mg/kg) ※ 정성만 가능한 물질은 ‘-’로 표시 [표 3]
고시 원문의 표기·오탈자·조판 잔재를 고치지 않고 그대로 옮겼습니다.
상 분류 C18USP L1 상당
약전 일반명 '액체크로마토그래프용옥타데실실릴실리카겔'(USP 분류로는 L1 상당)에 해당. 약전은 브랜드를 지정하지 않으므로 각조가 기재한 물리 사양(치수·입자경 등)과 KP 통칙·일반시험법의 조정 허용범위 안에서 해당 상을 충족하는 C18을 선택할 수 있다 — 선택 기준은 시스템적합성(분리도·테일링·RSD) 통과 용이성과 재현성이다.